CN114716657B - Nucleating agent, polypropylene resin, and preparation method and application thereof - Google Patents

Nucleating agent, polypropylene resin, and preparation method and application thereof Download PDF

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CN114716657B
CN114716657B CN202210514591.9A CN202210514591A CN114716657B CN 114716657 B CN114716657 B CN 114716657B CN 202210514591 A CN202210514591 A CN 202210514591A CN 114716657 B CN114716657 B CN 114716657B
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nucleating agent
phase
polypropylene resin
glycidyl ether
polypropylene
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CN114716657A (en
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任兴嘉
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Zhuozhou Juancheng Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/91Polymers modified by chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10Homopolymers or copolymers of propene
    • C08L23/12Polypropene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/24Crystallisation aids

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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Abstract

The invention provides a nucleating agent, polypropylene resin, a preparation method and application thereof, wherein the preparation method of the nucleating agent takes high internal phase emulsion as a system, the nucleating agent is generated by polymerization, and substances containing hydroxyl groups and substances containing carboxylate are dissolved in water to form a disperse phase; dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase; and adding the disperse phase into the continuous phase to perform polymerization reaction to obtain the nucleating agent. The prepared nucleating agent is long-fatty-chain chemically modified benzoate, the organic modification of sodium benzoate is realized by adopting a long-fatty-chain modification mode, and the compatibility of sodium benzoate in polypropylene is improved, so that the effect of the nucleating agent in polypropylene is effectively improved, and the nucleating agent has the function of obviously improving the flexural modulus of polypropylene when the nucleating agent is applied to polypropylene resin.

Description

Nucleating agent, polypropylene resin, and preparation method and application thereof
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a nucleating agent, polypropylene resin, a preparation method and application thereof.
Background
The nucleating agent is an auxiliary agent for incomplete crystallization plastics such as polyethylene, polypropylene and the like, and can play roles in shortening the forming period, improving the transparency, surface gloss, tensile strength, rigidity, heat distortion temperature, impact resistance, creep resistance and other physical and mechanical properties by changing the crystallization behavior of resin, accelerating crystallization rate, increasing crystallization density and promoting grain size refinement.
Sodium benzoate is used as a nucleating agent, can effectively improve the crystallinity and the crystallization temperature of polypropylene, and is a commonly used polypropylene nucleating agent. The dispersibility of sodium benzoate in polypropylene resins is often a bottleneck limiting the application of sodium benzoate nucleators. The particle size of sodium benzoate can be effectively reduced by jet milling, and the improvement effect on the nucleating agent effect is limited.
For example, chinese patent document CN102775616a discloses a method for improving the dispersibility of sodium benzoate/talc composite nucleating agent in polypropylene, which can uniformly disperse sodium benzoate in polypropylene resin, and improve the impact resistance of the product while improving the crystallization temperature. Chinese patent document CN102219927a discloses a composite nucleating agent comprising carboxylates and phosphates, which not only can significantly improve the flexural modulus and heat distortion temperature of polypropylene products, but also can significantly improve impact strength.
Although the above-mentioned mode can improve the effect of sodium benzoate nucleating agent to a certain extent, the improvement effect is limited, and when the nucleating agent is applied to polypropylene resin, the mechanical properties of the obtained high polymer material are still not ideal.
Disclosure of Invention
The invention aims to solve the technical problems of providing a nucleating agent, polypropylene resin, a preparation method and application thereof, and solves the problem that the mechanical properties of the sodium benzoate nucleating agent applied to the polypropylene resin in the prior art are not ideal.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the preparation method of the nucleating agent takes high internal phase emulsion as a system, and polymerizes to generate the nucleating agent, comprising the following steps:
dissolving a substance containing hydroxyl groups and a substance containing carboxylate in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase;
and adding the disperse phase into the continuous phase to perform polymerization reaction to obtain the nucleating agent.
Preferably, the disperse phase is added into the continuous phase in a dropwise manner; preferably, the dropping speed is 10-20ml/min.
Optionally, the reaction temperature of the polymerization reaction is 80 ℃ and the reaction time is 6-8h.
Further preferably, the preparation method of the nucleating agent further comprises: and after the polymerization reaction, washing the reaction product by adopting ethanol, and drying.
Further preferably, the temperature of the drying is 60-80 ℃ and the time is 8 hours.
Preferably, the substance containing hydroxyl groups is one or more of cellulose nanocrystals and beta-cyclodextrin;
the carboxylate-containing substance is one or more of sodium p-hydroxybenzoate and sodium 2-hydroxybenzoate.
The long fatty chain glycidyl ether is glycidyl ether with 12-14 carbon atoms;
the glycidyl ester monomer is one or more of glycidyl acrylate and triglycidyl isocyanurate;
the organic solvent is toluene solvent.
Further preferably, the mass ratio of the hydroxyl group-containing substance, the carboxylate-containing substance, and the water is (1-9): (10-40): 60.
further preferably, the mass ratio of the long fatty chain glycidyl ether, the glycidyl ester monomer, and the organic solvent is (10-30): (13-19): 70.
preferably, the dispersed phase is composed of cellulose nanocrystals, sodium parahydroxybenzoate and water;
the continuous phase is composed of the long fatty chain glycidyl ether, glycidyl acrylate, triglycidyl isocyanurate and toluene solvent.
Further preferably, the dispersed phase is prepared from cellulose nanocrystals, sodium p-hydroxybenzoate and water according to (1-9): (10-40): 60 by mass ratio.
Further preferably, the dispersed phase is prepared from cellulose nanocrystals, sodium p-hydroxybenzoate and water according to (3-5): (30-40): 60 by mass ratio.
Further preferably, the continuous phase is prepared from the long fatty chain glycidyl ether, glycidyl acrylate, triglycidyl isocyanurate and toluene solvent according to (10-30): 10: (3-9): 70 mass ratio.
Further preferably, the continuous phase is prepared from the long fatty chain glycidyl ether, glycidyl acrylate, triglycidyl isocyanurate and toluene solvent according to (20-30): 10: (3-5): 70 mass ratio.
Preferably, the volume fraction of the dispersed phase of the high internal phase emulsion is greater than or equal to 74%;
optionally, the high internal phase emulsion has a volume fraction of dispersed phase of 80% -90%;
optionally, the high internal phase emulsion has a volume fraction of dispersed phase of 80% to 85%.
Preferably, the polymerization reaction uses a nonionic surfactant as an emulsifier.
Further preferably, the nonionic surfactant is one or more of polyethylene glycol (200) monolaurate, glycerol monolaurate, polyglycerol fatty acid ester, polyethylene glycol (200) dilaurate, diglycerol monolaurate, sorbitol monolaurate, span 80;
further preferably, the nonionic surfactant is polyethylene glycol (200) monolaurate, polyethylene glycol (200) dilaurate, and span 80.
Further preferably, the mass ratio of the nonionic surfactant to the continuous phase is (0.8-1): 100.
further preferably, the polymerization is carried out under the action of a catalyst.
Further preferably, the catalyst is a tertiary amine.
Further preferably, the tertiary amine is one or more of dodecyl amine, dodecyl amine and octadecyl amine.
Further preferably, the mass ratio of the catalyst to the continuous phase is (0.5-0.9): 100.
further preferably, the mass ratio of the catalyst to the continuous phase is (0.5-0.7): 100.
the invention also provides a nucleating agent obtained by the preparation method of the nucleating agent.
The invention also provides a polypropylene resin, which is added with the nucleating agent.
Preferably, the concentration of the nucleating agent in the polypropylene resin is 1000 to 2000ppm.
The invention also provides application of the nucleating agent in the field of polypropylene resin materials.
The scheme of the invention at least comprises the following beneficial effects:
(1) The preparation method of the nucleating agent of the invention takes high internal phase emulsion as a system, generates the nucleating agent by polymerization, and dissolves substances containing hydroxyl groups and substances containing carboxylate into water to form a disperse phase; dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase; and adding the disperse phase into the continuous phase to perform polymerization reaction to obtain the nucleating agent. The prepared nucleating agent is long-fatty-chain chemically modified benzoate, the organic modification of sodium benzoate is realized by adopting a long-fatty-chain modification mode, and the compatibility of benzoate in polypropylene is improved, so that the effect of the nucleating agent in polypropylene is effectively improved, and the nucleating agent has the function of obviously improving the flexural modulus of polypropylene when the nucleating agent is applied to polypropylene resin.
Specifically, the nucleating agent of the benzoate is not matched with the melting point of the polypropylene, and has low compatibility with the polypropylene, when the polypropylene is melted and crystallized, the nucleating agent of the benzoate is dispersed in the polypropylene resin in a particle shape, so that the dispersion uniformity is poor, and when the polypropylene is induced to be crystallized, the formed spherulites have larger size, and further the obtained polypropylene material is brittle and has poor mechanical property. The long fatty chain glycidyl ether and glyceride monomers contained in the continuous phase of the invention contain epoxy groups, the substances containing hydroxyl groups in the disperse phase contain hydroxyl groups, and when the substances containing carboxylate are p-hydroxybenzoic acid sodium salt and/or 2-hydroxybenzoic acid sodium salt, the substances containing carboxylate also contain hydroxyl groups, and the epoxy groups can carry out ring-opening reaction on the hydroxyl groups to form benzoate with long fatty chain chemically modified, so that the obtained nucleating agent has proper compatibility with polypropylene. Compared with benzoate, the nucleating agent disclosed by the invention has a long fatty chain, has higher compatibility with polypropylene of a long-chain polymer, can be more uniformly dispersed in polypropylene resin, and cannot have too high compatibility with polypropylene, so that the nucleating agent is difficult to induce crystallization. As the nucleating agent has better dispersibility, more crystallization sites are formed when the polypropylene is melted and crystallized, and the formed spherulites have smaller size and are more compact, the obtained polypropylene material has better mechanical property and can reach higher flexural modulus.
(2) According to the preparation method of the nucleating agent, the nonionic surfactant is added as the emulsifier, so that the nucleating agent of the water-in-oil type high internal phase emulsion can be prepared. In particular, when the nonionic surfactant is polyethylene glycol (200) monolaurate, polyethylene glycol (200) dilaurate and span 80, the emulsion stability is better. In addition, tertiary amine is used as a catalyst, and the continuous phase and the disperse phase can undergo condensation reaction between oil-water interfaces under the action of the catalyst, so that the reaction time is shortened.
Detailed Description
The specific conditions not noted in the examples of the present invention were carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used are not marked for manufacturers, are conventional products which can be obtained through commercial purchase, and the implementation of the technical scheme and the realization of the technical effect of the invention are not influenced by raw materials of different manufacturers and models.
Example 1
The preparation method of the nucleating agent of the embodiment takes high internal phase emulsion as a system and polymerizes to form the nucleating agent, and comprises the following steps:
dissolving a substance containing hydroxyl groups and a substance containing carboxylate in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase;
and (3) dropwise adding the disperse phase into the continuous phase at the speed of 10ml/min, and carrying out polymerization reaction at the temperature of 70 ℃ for 8 hours to obtain the nucleating agent.
Wherein the volume ratio of the dispersed phase to the continuous phase is 74:26;
the mass ratio of the substance containing hydroxyl groups, the substance containing carboxylate and the water is 1:25:60.
the mass ratio of the long fatty chain glycidyl ether to the glycidyl ester monomer to the organic solvent is 10:16:70.
in this embodiment, the substance containing hydroxyl groups is cellulose nanocrystals; the carboxylate-containing material is sodium parahydroxybenzoate; the long fatty chain glycidyl ether is glycidyl ether with 12 carbon atoms; the glycidyl ester monomer is triglycidyl isocyanurate; the organic solvent is toluene solvent.
The polypropylene resin of the embodiment is added with the nucleating agent prepared by the method, and the concentration of the nucleating agent in the polypropylene resin is 1000ppm. The polypropylene resin may be a polypropylene T30S resin as a matrix, or may be a commercially available material of other specifications.
Example 2
The preparation method of the nucleating agent of the embodiment takes high internal phase emulsion as a system and polymerizes to form the nucleating agent, and comprises the following steps:
dissolving a substance containing hydroxyl groups and a substance containing carboxylate in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase;
and (3) dropwise adding the disperse phase into the continuous phase at a speed of 15ml/min, and carrying out polymerization reaction at a reaction temperature of 80 ℃ for 6 hours to obtain the nucleating agent.
Wherein the volume ratio of the dispersed phase to the continuous phase is 80:20, a step of;
the mass ratio of the substance containing hydroxyl groups, the substance containing carboxylate and the water is 9:40:60.
the mass ratio of the long fatty chain glycidyl ether to the glycidyl ester monomer to the organic solvent is 20:19:70.
in this embodiment, the substance containing hydroxyl groups is beta-cyclodextrin; the carboxylate-containing material is sodium 2-hydroxy benzoate; the long fatty chain glycidyl ether is glycidyl ether with 13 carbon atoms; the glycidyl ester monomer is glycidyl acrylate; the organic solvent is toluene solvent.
The polypropylene resin of the embodiment is added with the nucleating agent prepared by the method, and the concentration of the nucleating agent in the polypropylene resin is 2000ppm.
Example 3
The preparation method of the nucleating agent of the embodiment takes high internal phase emulsion as a system and polymerizes to form the nucleating agent, and comprises the following steps:
dissolving a substance containing hydroxyl groups and a substance containing carboxylate in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase;
and (3) dropwise adding the disperse phase into the continuous phase at a speed of 20ml/min, and carrying out polymerization reaction at a reaction temperature of 60 ℃ for 7 hours to obtain the nucleating agent.
Wherein the volume ratio of the dispersed phase to the continuous phase is 90:10;
the mass ratio of the substance containing hydroxyl groups, the substance containing carboxylate and the water is 5:10:60.
the mass ratio of the long fatty chain glycidyl ether to the glycidyl ester monomer to the organic solvent is 30:13:70.
in this embodiment, the substance containing hydroxyl groups is cellulose nanocrystals and β -cyclodextrin according to 1:1 weight ratio; the carboxylate-containing substance is sodium p-hydroxybenzoate and sodium 2-hydroxybenzoate according to the following formula 1:1 weight ratio; the long fatty chain glycidyl ether is glycidyl ether with 14 carbon atoms; the glycidyl ester monomer is formed by mixing acrylic acid glycidyl ester and triglycidyl isocyanurate according to the mass ratio of 1:1; the organic solvent is toluene solvent.
The polypropylene resin of the embodiment is added with the nucleating agent prepared by the method, and the concentration of the nucleating agent in the polypropylene resin is 1500ppm.
Example 4
The preparation method of the nucleating agent of the embodiment takes high internal phase emulsion as a system and polymerizes to form the nucleating agent, and comprises the following steps:
dissolving a substance containing hydroxyl groups, a substance containing carboxylate and a nonionic surfactant in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether, glycidyl ester monomer and catalyst in organic solvent to form continuous phase;
and (3) dropwise adding the disperse phase into the continuous phase at a speed of 20ml/min, and carrying out polymerization reaction at a reaction temperature of 60 ℃ for 7 hours to obtain the nucleating agent.
Wherein the volume ratio of the dispersed phase to the continuous phase is 82:18;
the mass ratio of the substance containing hydroxyl groups, the substance containing carboxylate and the water is 5:30:60.
the mass ratio of the long fatty chain glycidyl ether to the glycidyl ester monomer to the organic solvent is 25:13:70.
the mass ratio of the nonionic surfactant to the continuous phase was 0.9:100.
the mass ratio of the catalyst to the continuous phase was 0.5:100.
in this embodiment, the substance containing hydroxyl groups is cellulose nanocrystals; the carboxylate-containing material is sodium parahydroxybenzoate; the long fatty chain glycidyl ether is glycidyl ether with 14 carbon atoms; the glycidyl ester monomer is formed by mixing acrylic acid glycidyl ester and triglycidyl isocyanurate according to the mass ratio of 10:3; the organic solvent is toluene solvent. The nonionic surfactant is formed by mixing polyethylene glycol (200) monolaurate, polyethylene glycol (200) dilaurate and span 80 according to the mass ratio of 1:1:1. The catalyst is tertiary amine, and the tertiary amine is dodecyl amine.
The polypropylene resin of the embodiment is added with the nucleating agent prepared by the method, and the concentration of the nucleating agent in the polypropylene resin is 2000ppm.
Example 5
The preparation method of the nucleating agent of the embodiment takes high internal phase emulsion as a system and polymerizes to form the nucleating agent, and comprises the following steps:
dissolving a substance containing hydroxyl groups, a substance containing carboxylate and a nonionic surfactant in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether, glycidyl ester monomer and catalyst in organic solvent to form continuous phase;
and (3) dropwise adding the disperse phase into the continuous phase at a speed of 20ml/min, and carrying out polymerization reaction at a reaction temperature of 60 ℃ for 7 hours to obtain the nucleating agent.
Wherein the volume ratio of the dispersed phase to the continuous phase is 85:15;
the mass ratio of the substance containing hydroxyl groups, the substance containing carboxylate and the water is 3:40:60.
the mass ratio of the long fatty chain glycidyl ether to the glycidyl ester monomer to the organic solvent is 30:14:70.
the mass ratio of the nonionic surfactant to the continuous phase was 0.8:100.
the mass ratio of the catalyst to the continuous phase was 0.9:100.
in this embodiment, the substance containing hydroxyl groups is cellulose nanocrystals; the carboxylate-containing material is sodium parahydroxybenzoate; the long fatty chain glycidyl ether is glycidyl ether with 14 carbon atoms; the glycidyl ester monomer is formed by mixing acrylic acid glycidyl ester and triglycidyl isocyanurate according to the mass ratio of 10:4; the organic solvent is toluene solvent. The nonionic surfactant is formed by mixing polyethylene glycol (200) monolaurate, polyethylene glycol (200) dilaurate and span 80 according to the mass ratio of 1:1:1. The catalyst is tertiary amine, and the tertiary amine is dodecyl amine.
The polypropylene resin of the embodiment is added with the nucleating agent prepared by the method, and the concentration of the nucleating agent in the polypropylene resin is 2000ppm.
Example 6
The preparation method of the nucleating agent of the embodiment takes high internal phase emulsion as a system and polymerizes to form the nucleating agent, and comprises the following steps:
dissolving a substance containing hydroxyl groups, a substance containing carboxylate and a nonionic surfactant in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether, glycidyl ester monomer and catalyst in organic solvent to form continuous phase;
and (3) dropwise adding the disperse phase into the continuous phase at a speed of 20ml/min, and carrying out polymerization reaction at a reaction temperature of 60 ℃ for 7 hours to obtain the nucleating agent.
Wherein the volume ratio of the dispersed phase to the continuous phase is 85:15;
the mass ratio of the substance containing hydroxyl groups, the substance containing carboxylate and the water is 4:35:60.
the mass ratio of the long fatty chain glycidyl ether to the glycidyl ester monomer to the organic solvent is 20:15:70.
the mass ratio of the nonionic surfactant to the continuous phase is 1:100.
the mass ratio of the catalyst to the continuous phase was 0.7:100.
in this embodiment, the substance containing hydroxyl groups is cellulose nanocrystals; the carboxylate-containing material is sodium parahydroxybenzoate; the long fatty chain glycidyl ether is glycidyl ether with 14 carbon atoms; the glycidyl ester monomer is formed by mixing acrylic acid glycidyl ester and triglycidyl isocyanurate according to the mass ratio of 10:5; the organic solvent is toluene solvent. The nonionic surfactant is formed by mixing polyethylene glycol (200) monolaurate, polyethylene glycol (200) dilaurate and span 80 according to the mass ratio of 1:1:1. The catalyst is tertiary amine, and the tertiary amine is dodecyl amine.
The polypropylene resin of the embodiment is added with the nucleating agent prepared by the method, and the concentration of the nucleating agent in the polypropylene resin is 2000ppm.
Example 7
The same raw materials and preparation methods as in example 6 were used in this example, except that: the long fatty chain glycidyl ether is glycidyl ether with 15 carbon atoms.
Example 8
The same raw materials and preparation methods as in example 6 were used in this example, except that: the long fatty chain glycidyl ether is glycidyl ether with the number of carbon atoms of 11.
Comparative example 1
The polypropylene resin of this comparative example was added with sodium benzoate as a nucleating agent, and the concentration of sodium benzoate nucleating agent in the polypropylene resin was 2000ppm.
Effect comparative example
To verify the technical effect of the nucleating agent of the present invention, the following tests were performed:
the polypropylene resins prepared in examples 1 to 8 and comparative example 1 were injection molded into dumbbell-shaped bars of the same size by melt extrusion using a twin screw extruder at 200℃and tested for flexural modulus according to the method described in GB/T9341-2000.
The results are as follows:
sequence number Flexural modulus (MPa)
Example 1 1810
Example 2 1870
Example 3 1956
Example 4 2013
Example 5 2060
Example 6 2156
Example 7 1794
Example 8 1736
Comparative example 1 1715
In the above results, the higher the flexural modulus, the better the mechanical properties of the polypropylene resin material. From the above results, it is clear that the nucleating agent of the present invention can significantly improve the mechanical properties of polypropylene resin materials and achieve a higher flexural modulus when used in polypropylene resins. Further, it is understood from the comparison of examples 1 to 8 that a preferable effect can be obtained when the long fatty chain glycidyl ether is a glycidyl ether having 12 to 14 carbon atoms, wherein the mechanical properties of the polypropylene resin material of example 6 are optimal. In examples 7-8, when the number of carbon atoms is too large or too small, the compatibility of the nucleating agent with polypropylene is affected, and the mechanical properties of the obtained polypropylene material are slightly inferior.
It will be appreciated by those skilled in the art that the present invention can be carried out in other embodiments without departing from the spirit or essential characteristics thereof. Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.

Claims (12)

1. The preparation method of the nucleating agent is characterized in that the nucleating agent is polymerized by taking high internal phase emulsion as a system, and comprises the following steps:
dissolving a substance containing hydroxyl groups and a substance containing carboxylate in water to form a dispersed phase;
dissolving long fatty chain glycidyl ether and glycidyl ester monomer in an organic solvent to form a continuous phase;
adding the disperse phase into the continuous phase for polymerization reaction to obtain a nucleating agent;
wherein the substance containing hydroxyl groups is one or more of cellulose nanocrystalline and beta-cyclodextrin;
the carboxylate-containing substance is one or more of sodium p-hydroxybenzoate and sodium 2-hydroxybenzoate;
the long fatty chain glycidyl ether is glycidyl ether with 12-14 carbon atoms;
the glycidyl ester monomer is one or more of glycidyl acrylate and triglycidyl isocyanurate.
2. The method of preparing a nucleating agent according to claim 1, wherein said dispersed phase is added to said continuous phase by means of dropping;
optionally, the reaction temperature of the polymerization reaction is 60-80 ℃ and the reaction time is 6-8h.
3. The method for producing a nucleating agent according to claim 1, wherein said organic solvent is a toluene solvent.
4. A method of preparing a nucleating agent according to claim 3, wherein said dispersed phase is composed of cellulose nanocrystals, sodium parahydroxybenzoate and water;
the continuous phase is composed of the long fatty chain glycidyl ether, glycidyl acrylate, triglycidyl isocyanurate and toluene solvent.
5. The method of preparing a nucleating agent according to claim 1, wherein the volume fraction of the dispersed phase of said high internal phase emulsion is greater than or equal to 74%.
6. The method of claim 5, wherein the high internal phase emulsion has a dispersed phase volume fraction of 80% to 90%.
7. The method of preparing a nucleating agent according to claim 6, wherein optionally the volume fraction of the dispersed phase of said high internal phase emulsion is 80% to 85%.
8. The method of preparing a nucleating agent as defined in claim 1, wherein the polymerization reaction uses a nonionic surfactant as an emulsifier.
9. A nucleating agent obtainable by the process for the preparation of a nucleating agent as claimed in any one of claims 1 to 8.
10. A polypropylene resin to which the nucleating agent of claim 9 is added.
11. The polypropylene resin according to claim 10, wherein the concentration of the nucleating agent in the polypropylene resin is 1000 to 2000ppm.
12. Use of the nucleating agent of claim 9 in the field of polypropylene resin materials.
CN202210514591.9A 2022-05-11 2022-05-11 Nucleating agent, polypropylene resin, and preparation method and application thereof Active CN114716657B (en)

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CN101845171A (en) * 2010-04-20 2010-09-29 广州呈和科技有限公司 Polypropylene reinforcement nucleating agent composition
CN103788472B (en) * 2012-10-30 2016-09-21 中国石油化工股份有限公司 A kind of binary composite polypropylene nucleator, preparation method and application
PT2883925T (en) * 2013-12-12 2017-01-02 Repsol Sa Polypropylene based composition
CN112080008A (en) * 2020-09-25 2020-12-15 华东理工大学 Cage type silsesquioxane phosphate nucleating agent and preparation method and application thereof
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