CN111073027A - High-temperature-resistant thermal expansion type foaming microcapsule and preparation method thereof - Google Patents
High-temperature-resistant thermal expansion type foaming microcapsule and preparation method thereof Download PDFInfo
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- CN111073027A CN111073027A CN201911402396.1A CN201911402396A CN111073027A CN 111073027 A CN111073027 A CN 111073027A CN 201911402396 A CN201911402396 A CN 201911402396A CN 111073027 A CN111073027 A CN 111073027A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/44—Acrylonitrile
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/22—Expandable microspheres, e.g. Expancel®
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Abstract
The invention belongs to the field of foaming microcapsules, in particular to a high-temperature-resistant thermal expansion type foaming microcapsule and a preparation method thereof, aiming at the problems that the existing prepared low-temperature thermal expansion type microcapsule powder is applied to different fields, but the application in the high-temperature field has a plurality of defects, the following scheme is provided, wherein the preparation method of the high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps: s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition; s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.01 wt% -0.1 wt% of a cross-linking agent, 5 wt% -15 wt% of an initiator and 40 wt% -50 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil phase mixed solution. The shell is crosslinked with the shell by using the specific crosslinking agent, so that the high-temperature resistance of the wall material is greatly improved.
Description
Technical Field
The invention relates to the technical field of foaming microcapsules, in particular to a high-temperature-resistant thermal expansion type foaming microcapsule and a preparation method thereof.
Background
The high-temperature thermal expansion type microcapsule is a microsphere taking a thermoplastic polymer as a shell and a foaming agent with a higher boiling point as a capsule core, the polymer shell is softened along with the rise of temperature, the foaming agent with a lower boiling point is gasified, so that the microcapsule expands, and when the bearing pressure of the shell is equal to the gasification expansion pressure value of the capsule core, the expansion of the microcapsule is finished, so that the foaming microsphere is formed.
The high-temperature thermal expansion type foaming microcapsule can be used in the fields of high-temperature phase change heat exchange materials, insulating material lightweight materials and the like. In recent years, the technology of low-temperature microcapsules and the preparation process thereof are reported in patents such as US6509348, CN105555851A, CN108219182A and the like, and the prepared low-temperature thermal expansion type microcapsule powder is applied to different fields, but the application in the high-temperature field has a plurality of defects.
Disclosure of Invention
The invention aims to solve the problems that the low-temperature thermal expansion type microcapsule powder prepared in the prior art is applied to different fields, but the application in the high-temperature field has a plurality of defects, and provides a high-temperature resistant thermal expansion type foaming microcapsule and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-temperature-resistant thermal expansion type foaming microcapsule comprises a foaming agent core and a microcapsule shell, wherein the foaming agent core is low-boiling-point aliphatic alkane, and the microcapsule shell is formed by the action of a monomer with high crosslinking degree and a specific initiator.
Preferably, the particle size of the microcapsule shell is 1-50 um.
Preferably, the monomer consists of acrylate and acrylonitrile, and the initiator is an acrylate initiator.
A preparation method of a high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.01 wt% -0.1 wt% of a cross-linking agent, 5 wt% -15 wt% of an initiator and 40 wt% -50 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension liquid in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
Preferably, in the S2, the total weight of the double-bond organic substance is 100 wt% as a calculation standard, and the double-bond organic substance includes 35 to 55 wt% of hydroxypropyl acrylate monomer, 40 to 55 wt% of acrylonitrile, and 0.5 to 2 wt% of azobisisobutyronitrile.
Preferably, in S4, the temperature of the reaction kettle is set to be 60-70 ℃, the time of the reaction kettle is set to be 15-25h, and the stirring speed of the reaction kettle is set to be 500-700 r/min.
Preferably, in the S4, it is required to remove the monomer residue in the white suspension containing the thermally expandable microcapsule.
Preferably, in the step S5, the suction filtration time is set to be 2-3 h.
According to the high-temperature-resistant thermal expansion type foaming microcapsule and the preparation method thereof, the shells are mutually crosslinked by using the specific crosslinking agent, so that the high-temperature resistance of the wall material is greatly improved, and the aim of preparing the high-temperature-resistant thermal expansion type foaming microcapsule is fulfilled.
The shell is crosslinked with the shell by using the specific crosslinking agent, so that the high-temperature resistance of the wall material is greatly improved.
Drawings
Fig. 1 is a schematic structural diagram of a high-temperature resistant thermal expansion type foaming microcapsule provided by the invention.
In the figure: 1. a blowing agent core; 2. and (4) microcapsule shells.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
Referring to fig. 1, the high temperature resistant thermal expansion type foaming microcapsule comprises a foaming agent core 1 and a microcapsule shell 2, wherein the foaming agent core 1 is low boiling point aliphatic alkane, and the microcapsule shell 2 is formed by the action of a monomer with high crosslinking degree and a specific initiator.
In this embodiment, the particle size of the microcapsule shell 2 is 1 to 50 um.
In this embodiment, the monomer is composed of acrylates and acrylonitriles, and the initiator is an acrylate initiator.
A preparation method of a high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.01 wt% of a cross-linking agent, 5 wt% of an initiator and 40 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil-phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
In S2, the total weight of the double-bond organic matter is 100 wt% as a calculation standard, hydroxypropyl acrylate monomer accounts for 35 wt% of the double-bond organic matter, acrylonitrile accounts for 40 wt%, azobisisobutyronitrile accounts for 0.5 wt%, in S4, the temperature of the reaction kettle is set to be 60 ℃, the time of the reaction kettle is set to be 15 hours, the stirring speed of the reaction kettle is set to be 500r/min, in S4, the monomer residue in the white suspension containing the thermal expansion microcapsules needs to be removed, and in S5, the suction filtration time is set to be 2 hours.
Example two
Referring to fig. 1, the high temperature resistant thermal expansion type foaming microcapsule comprises a foaming agent core 1 and a microcapsule shell 2, wherein the foaming agent core 1 is low boiling point aliphatic alkane, and the microcapsule shell 2 is formed by the action of a monomer with high crosslinking degree and a specific initiator.
In this embodiment, the particle size of the microcapsule shell 2 is 1 to 50 um.
In this embodiment, the monomer is composed of acrylates and acrylonitriles, and the initiator is an acrylate initiator.
A preparation method of a high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.02 wt% of a cross-linking agent, 7 wt% of an initiator and 42 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil-phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
In S2, the total weight of double-bond organic matters is 100 wt% as a calculation standard, hydroxypropyl acrylate monomer accounts for 37 wt% in the double-bond organic matters, acrylonitrile accounts for 42 wt%, azobisisobutyronitrile accounts for 0.7 wt%, in S4, the temperature of a reaction kettle is set to be 62 ℃, the time of the reaction kettle is set to be 17 hours, the stirring speed of the reaction kettle is set to be 540r/min, in S4, the monomer residues in the white suspension containing the thermal expansion microcapsules are required to be removed, and in S5, the suction filtration time is set to be 2 hours.
EXAMPLE III
Referring to fig. 1, the high temperature resistant thermal expansion type foaming microcapsule comprises a foaming agent core 1 and a microcapsule shell 2, wherein the foaming agent core 1 is low boiling point aliphatic alkane, and the microcapsule shell 2 is formed by the action of a monomer with high crosslinking degree and a specific initiator.
In this embodiment, the particle size of the microcapsule shell 2 is 1 to 50 um.
In this embodiment, the monomer is composed of acrylates and acrylonitriles, and the initiator is an acrylate initiator.
A preparation method of a high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.04 wt% of a cross-linking agent, 10 wt% of an initiator and 44 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil-phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
In S2, the total weight of double-bond organic matters is 100 wt% as a calculation standard, hydroxypropyl acrylate monomer accounts for 40 wt% of the double-bond organic matters, acrylonitrile accounts for 50 wt%, azobisisobutyronitrile accounts for 1 wt%, in S4, the temperature of a reaction kettle is set to be 66, the time of the reaction kettle is set to be 20 hours, the stirring speed of the reaction kettle is set to be 600r/min, in S4, the monomer residues in the white suspension containing the thermal expansion microcapsules need to be removed, and in S5, the suction filtration time is set to be 2 hours.
Example four
Referring to fig. 1, the high temperature resistant thermal expansion type foaming microcapsule comprises a foaming agent core 1 and a microcapsule shell 2, wherein the foaming agent core 1 is low boiling point aliphatic alkane, and the microcapsule shell 2 is formed by the action of a monomer with high crosslinking degree and a specific initiator.
In this embodiment, the particle size of the microcapsule shell 2 is 1 to 50 um.
In this embodiment, the monomer is composed of acrylates and acrylonitriles, and the initiator is an acrylate initiator.
A preparation method of a high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.08 wt% of a cross-linking agent, 12 wt% of an initiator and 48 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil-phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
In S2, the total weight of the double-bond organic matter is 100 wt% as a calculation standard, hydroxypropyl acrylate monomer accounts for 52 wt% in the double-bond organic matter, acrylonitrile accounts for 52 wt%, azobisisobutyronitrile accounts for 1.5 wt%, in S4, the temperature of the reaction kettle is set to 68, the time of the reaction kettle is set to 22 hours, the stirring speed of the reaction kettle is set to 650r/min, in S4, the monomer residue in the white suspension containing the thermal expansion microcapsules needs to be removed, and in S5, the suction filtration time is set to 3 hours.
EXAMPLE five
Referring to fig. 1, the high temperature resistant thermal expansion type foaming microcapsule comprises a foaming agent core 1 and a microcapsule shell 2, wherein the foaming agent core 1 is low boiling point aliphatic alkane, and the microcapsule shell 2 is formed by the action of a monomer with high crosslinking degree and a specific initiator.
In this embodiment, the particle size of the microcapsule shell 2 is 1 to 50 um.
In this embodiment, the monomer is composed of acrylates and acrylonitriles, and the initiator is an acrylate initiator.
A preparation method of a high-temperature-resistant thermal expansion type foaming microcapsule comprises the following steps:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.1 wt% of a cross-linking agent, 15 wt% of an initiator and 50 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil-phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
In S2, the total weight of double-bond organic matters is 100 wt% as a calculation standard, hydroxypropyl acrylate monomer accounts for 55 wt% in the double-bond organic matters, acrylonitrile accounts for 55 wt%, azobisisobutyronitrile accounts for 2 wt%, in S4, the temperature of a reaction kettle is set to be 70 ℃, the time of the reaction kettle is set to be 25 hours, the stirring speed of the reaction kettle is set to be 700r/min, in S4, the monomer residues in the white suspension containing the thermal expansion microcapsules need to be removed, and in S5, the suction filtration time is set to be 3 hours.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A high-temperature-resistant thermal expansion type foaming microcapsule comprises a foaming agent core (1) and a microcapsule shell (2), and is characterized in that the foaming agent core (1) is low-boiling-point aliphatic alkane, and the microcapsule shell (2) is formed by the action of a monomer with high crosslinking degree and a specific initiator.
2. A high temperature resistant thermally intumescent foaming microcapsule according to claim 1 wherein the particle size of the microcapsule shell (2) is 1-50 um.
3. The high temperature resistant thermally intumescent foaming microcapsule according to claim 1, characterized in that said monomer is composed of acrylates and acrylonitriles and said initiator is an acrylate initiator.
4. The process for preparing high temperature resistant thermally expansive foamed microcapsules according to claim 1, comprising the steps of:
s1: preparing a water phase: adding an emulsifier, a suspending agent, inorganic salt and a polymerization inhibitor into deionized water and dispersing to obtain a water-phase composition;
s2: preparing an oil phase: taking the total weight of the double-bond organic matters as 100 wt% as a calculation reference, adding 0.01 wt% -0.1 wt% of a cross-linking agent, 5 wt% -15 wt% of an initiator and 40 wt% -50 wt% of a low-boiling-point foaming agent into the double-bond organic matters, and uniformly stirring to prepare an oil phase mixed solution;
s3: preparing a dispersion liquid: adding the water-phase composition obtained in the step S1 and the oil-phase mixed solution obtained in the step S2 into a mixer for mixing treatment, and obtaining a dispersion liquid after mixing;
s4: polymerization reaction: adding the dispersion liquid in the S3 into a reaction kettle for polymerization reaction to obtain a white suspension containing the thermal expansion microcapsules;
s5: and (3) suction filtration, washing and drying: and (4) carrying out suction filtration and washing on the white suspension liquid in the S4 to obtain the high-temperature-resistant thermal expansion type foaming microcapsule.
5. The method for preparing the high-temperature-resistant thermal expansion type foaming microcapsule according to claim 4, wherein in S2, the total weight of the double-bond organic substances is 100 wt% as a calculation standard, and the double-bond organic substances comprise 35-55 wt% of hydroxypropyl acrylate monomer, 40-55 wt% of acrylonitrile and 0.5-2 wt% of azobisisobutyronitrile.
6. The method as claimed in claim 4, wherein in S4, the temperature of the reaction kettle is set to 60-70 ℃, the time of the reaction kettle is set to 15-25h, and the stirring speed of the reaction kettle is set to 500-700 r/min.
7. The process for preparing high temperature resistant thermally expansive foamed microcapsule according to claim 4, wherein in said S4, it is necessary to remove monomer residues in the white suspension containing the thermally expansive microcapsules.
8. The process for preparing high temperature resistant thermally expansive foamed microcapsule according to claim 4, wherein in S5, the suction filtration time is set to 2-3 h.
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| CN114752141A (en) * | 2022-05-10 | 2022-07-15 | 杜章辉 | High-strength labor protection shoe sole and shoe sole production process |
| CN115368695A (en) * | 2022-08-08 | 2022-11-22 | 贵州师范大学 | Functional thermal expansion type foaming microcapsule and preparation method and application thereof |
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| CN114752141A (en) * | 2022-05-10 | 2022-07-15 | 杜章辉 | High-strength labor protection shoe sole and shoe sole production process |
| CN115368695A (en) * | 2022-08-08 | 2022-11-22 | 贵州师范大学 | Functional thermal expansion type foaming microcapsule and preparation method and application thereof |
| CN115368695B (en) * | 2022-08-08 | 2023-09-19 | 贵州师范大学 | Application method of functional thermal expansion type foaming microcapsule |
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Application publication date: 20200428 |