CN113788977B - Preparation method of flexible porous material - Google Patents
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/0066—Use of inorganic compounding ingredients
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08J2205/00—Foams characterised by their properties
- C08J2205/06—Flexible foams
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08J2325/00—Characterised by the use of homopolymers or 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; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- 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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
Abstract
The invention provides a preparation method of a flexible porous material, which comprises the following steps: s1, adding 2-6 parts of surfactant and 1-3 parts of first stabilizer into 30-40 parts of deionized water to prepare homogeneous aqueous solution serving as a water phase; preparing homogeneous oil solution as oil phase with resin 5-20 weight portions, propylene-styrene-butadiene copolymer 4-7 weight portions, the second stabilizer 1-3 weight portions, cell structure controlling agent 3-5 weight portions, promoter 1-4 weight portions and diluent 10-20 weight portions; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method; s2, polymerizing the prepared emulsion, and filtering, washing and drying to obtain the flexible porous material. According to the preparation method of the flexible porous material, the average particle size of the prepared foam microporous material is controllable, the cell structure is regular, the compression resilience is good, the flexibility is good, and the stability is excellent.
Description
Technical Field
The invention relates to the technical field of porous materials, in particular to a preparation method of a flexible porous material.
Background
The human body protection material is an auxiliary prevention and protection article for reducing or avoiding injury, accidents and occupational hazards of personnel in the life, production or working process, for example: the intake of particles, dust, bacteria and harmful gases is avoided, and the mask of a respiratory system is protected; earplugs or earmuffs to prevent noise from causing hearing damage; chemical protective clothing for preventing skin damage caused by toxic and harmful chemicals, particles, spray and the like; thermal clothes with special working environments such as heat insulation, heat preservation and waterproof functions belong to human body protection materials. Common human body protection materials are made into masks by adopting melt-blown high polymer fibers, earplugs are made of high-elastic silica gel, foam, polyester materials and the like, and protective clothing is made of high polymer materials such as silk fabric, double-side coated flame-retardant PVC, coated butyl rubber, coated chloroprene rubber and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the flexible pore material, which can improve the compression resilience and flexibility of the flexible pore material. The technical scheme adopted by the invention is as follows:
a method of preparing a flexible porous material, wherein: the method comprises the following steps:
s1, adding 2-6 parts of surfactant and 1-3 parts of first stabilizer into 30-40 parts of deionized water to prepare homogeneous aqueous solution serving as a water phase; preparing 5-20 parts of resin, 4-7 parts of propylene-styrene-butadiene copolymer, 1-3 parts of second stabilizer, 3-5 parts of cell structure control agent, 1-4 parts of accelerant and 10-20 parts of diluent into homogeneous oil solution serving as an oil phase; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method;
s2, polymerizing the prepared emulsion, and filtering, washing and drying to obtain the flexible porous material.
The propylene-styrene-butadiene copolymer is combined with the resin, so that the stability and the flexibility of the flexible pore material are further improved, and meanwhile, the toughness of the interior of the flexible pore material can be obviously improved, so that the strength of the flexible pore material in a severe environment for a long time is improved; through the combined use of the first stabilizer and the second stabilizer, the pores of the flexible microporous material are fine and uniform, foam collapse is prevented, and the thermal stability of the flexible microporous material is improved.
Preferably, the preparation method of the flexible porous material comprises the following steps: the surfactant of the step S1 is one or more of lauroyl glutamic acid, diethanolamide stearic acid monoglyceride and cocoyl diethanolamide.
Preferably, the preparation method of the flexible porous material comprises the following steps: the step S1 first stabilizer comprises 40 to 55wt% of Ba/Zn complex stabilizer and 25 to 30wt% of polyether triol and 15 to 35wt% of polyoxyethylene-polyoxypropylene copolymer.
Preferably, the preparation method of the flexible porous material comprises the following steps: the resin in the step S1 is one or more of polyurethane, polystyrene, polyvinyl chloride, polyethylene, polypropylene and phenolic resin.
Preferably, the preparation method of the flexible porous material comprises the following steps: the second stabilizer of the step S1 comprises 55-60 wt% of tert-butyl peroxy-2-ethylhexanoate and 40-45 wt% of calcium ricinoleate.
Preferably, the preparation method of the flexible porous material comprises the following steps: the step S1 is that the cell structure control agent is one or more of sodium carbonate, barium carbonate, zirconium phosphate and zinc carbonate.
Preferably, the preparation method of the flexible porous material comprises the following steps: the step S1 accelerant is graphene oxide.
Preferably, the preparation method of the flexible porous material comprises the following steps: the diluent in the step S1 is one or more of n-hexane, methyl ethyl ketone, acetone or isopropanol.
Preferably, the preparation method of the flexible porous material comprises the following steps: the polymerization temperature of the step S2 is 60-120 ℃, and the curing reaction time is 8-16h.
Preferably, the preparation method of the flexible porous material comprises the following steps: and in the step S2, the drying temperature is 60-80 ℃, and the drying time is 15-20h.
The invention has the advantages that:
(1) According to the preparation method of the flexible porous material, the average particle size of the prepared foam microporous material is controllable, the pore structure is regular, the compression resilience is good, the flexibility is good, and the stability is excellent.
(2) According to the preparation method of the flexible pore material, the propylene-styrene-butadiene copolymer is combined with the resin, so that the stability and the flexibility of the flexible pore material are further improved, and meanwhile, the toughness of the interior of the flexible pore material can be obviously improved, so that the strength of the flexible pore material in a severe environment for a long time is improved; the first stabilizer and the second stabilizer are combined for use, so that the pores of the flexible microporous material are fine and uniform, foam collapse is prevented, and the thermal stability of the flexible microporous material is improved.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
A method of preparing a flexible porous material, wherein: the method comprises the following steps:
s1, adding 2 parts of surfactant and 1 part of first stabilizer into 30 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing 5 parts of resin, 4 parts of propylene-styrene-butadiene copolymer, 1 part of second stabilizer, 3 parts of cell structure control agent, 1 part of accelerant and 10 parts of diluent into homogeneous oil solution serving as an oil phase; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogenizing emulsification, stirring or ultrasonic method; the surfactant is lauroyl glutamic acid; the first stabilizer comprises 40wt% Ba/Zn composite stabilizer and 25wt% polyether triol and 35wt% polyoxyethylene-polyoxypropylene copolymer; the resin is polyurethane; the second stabilizer comprises 55wt% of tert-butyl peroxy-2-ethylhexanoate and 45wt% of calcium ricinoleate; the foam structure control agent is sodium carbonate; the accelerant is graphene oxide; the diluent is n-hexane;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 60 ℃, the curing reaction time is 16h, filtering, washing and drying are carried out, the drying temperature is 60 ℃, and the drying time is 20h, so that the flexible pore material is finally obtained.
Example 2
A method of preparing a flexible porous material, wherein: the method comprises the following steps:
s1, adding 4 parts of surfactant and 2 parts of first stabilizer into 32 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing a homogeneous oil solution serving as an oil phase from 10 parts of resin, 5 parts of propylene-styrene-butadiene copolymer, 2 parts of a second stabilizer, 4 parts of a cell structure control agent, 2 parts of an accelerant and 15 parts of a diluent; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogenizing emulsification, stirring or ultrasonic method; the surfactant is diethanolamide stearic acid monoglyceride; the first stabilizer comprises 50wt% of Ba/Zn complex stabilizer and 26wt% of polyether triol and 24wt% of polyoxyethylene-polyoxypropylene copolymer; the resin is polystyrene; the second stabilizer comprises 58wt% of tert-butyl 2-ethylhexoate peroxide and 42wt% of calcium ricinoleate; the foam cell structure control agent is zirconium phosphate; the accelerant is graphene oxide; the diluent is methyl ethyl ketone;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 100 ℃, the curing reaction time is 10h, filtering, washing and drying are carried out, the drying temperature is 70 ℃, and the drying time is 18h, so that the flexible pore material is finally obtained.
Example 3
A method of preparing a flexible pore material, wherein: the method comprises the following steps:
s1, adding 6 parts of surfactant and 3 parts of first stabilizer into 40 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing 20 parts of resin, 7 parts of propylene-styrene-butadiene copolymer, 3 parts of second stabilizer, 5 parts of cell structure control agent, 4 parts of accelerant and 20 parts of diluent into homogeneous oil solution serving as an oil phase; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method; the surfactant is cocoyl diethanolamide, the first stabilizer comprises 55wt% of a ba/Zn complex stabilizer and 30wt% of a polyether triol and 15wt% of a polyoxyethylene-polyoxypropylene copolymer, the resin is polyethylene, the second stabilizer comprises 60wt% of t-butyl 2-ethylhexoate and 40wt% of calcium ricinoleate, the cell structure controlling agent is zinc carbonate, the accelerator is graphene oxide, and the diluent is isopropanol;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 120 ℃, the curing reaction time is 8h, filtering, washing and drying are carried out, the drying temperature is 80 ℃, and the drying time is 15h, so that the flexible porous material is finally obtained.
Comparative example 1
A method of preparing a flexible porous material, wherein: the method comprises the following steps:
s1, adding 2 parts of surfactant and 1 part of first stabilizer into 30 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing homogeneous oil solution as oil phase from 5 parts of resin, 4 parts of propylene-styrene-butadiene copolymer, 1 part of second stabilizer, 3 parts of cell structure control agent, 1 part of accelerant and 10 parts of diluent; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method; the surfactant is lauroyl glutamic acid; the first stabilizer is a Ba/Zn composite stabilizer; the resin is polyurethane; the second stabilizer comprises 55wt% of tert-butyl 2-ethylhexanoate peroxide and 45wt% of calcium ricinoleate; the foam structure control agent is sodium carbonate; the accelerant is graphene oxide; the diluent is n-hexane;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 60 ℃, the curing reaction time is 16h, filtering, washing and drying are carried out, the drying temperature is 60 ℃, and the drying time is 20h, so that the flexible pore material is finally obtained.
Comparative example 2
A method of preparing a flexible porous material, wherein: the method comprises the following steps:
s1, adding 2 parts of surfactant and 1 part of first stabilizer into 30 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing homogeneous oil solution as oil phase from 5 parts of resin, 4 parts of propylene-styrene-butadiene copolymer, 1 part of second stabilizer, 3 parts of cell structure control agent, 1 part of accelerant and 10 parts of diluent; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogenizing emulsification, stirring or ultrasonic method; the surfactant is lauroyl glutamic acid; the first stabilizer comprises 40wt% of Ba/Zn composite stabilizer and 25wt% of polyether triol and 35wt% of polyoxyethylene-polyoxypropylene copolymer; the resin is polyurethane; the second stabilizer is tert-butyl peroxy-2-ethyl hexanoate; the foam structure control agent is sodium carbonate; the accelerant is graphene oxide; the diluent is n-hexane;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 60 ℃, the curing reaction time is 16h, filtering, washing and drying are carried out, the drying temperature is 60 ℃, and the drying time is 20h, so that the flexible pore material is finally obtained.
Comparative example 3
A method of preparing a flexible pore material, wherein: the method comprises the following steps:
s1, adding 4 parts of surfactant and 2 parts of first stabilizer into 32 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing a homogeneous oil solution serving as an oil phase from 10 parts of resin, 5 parts of propylene-styrene-butadiene copolymer, 2 parts of a second stabilizer, 2 parts of an accelerant and 15 parts of a diluent; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method; the surfactant is diethanolamide stearic acid monoglyceride; the first stabilizer comprises 50wt% of Ba/Zn complex stabilizer and 26wt% of polyether triol and 24wt% of polyoxyethylene-polyoxypropylene copolymer; the resin is polystyrene; the second stabilizer comprises 58wt% of tert-butyl 2-ethylhexoate peroxide and 42wt% of calcium ricinoleate; the accelerant is graphene oxide; the diluent is methyl ethyl ketone;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 100 ℃, the curing reaction time is 10h, filtering, washing and drying are carried out, the drying temperature is 70 ℃, and the drying time is 18h, so that the flexible pore material is finally obtained.
Comparative example 4
A method of preparing a flexible porous material, wherein: the method comprises the following steps:
s1, adding 4 parts of surfactant and 2 parts of first stabilizer into 32 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing a homogeneous oil solution serving as an oil phase from 10 parts of resin, 5 parts of propylene-styrene-butadiene copolymer, 2 parts of a second stabilizer, 4 parts of a cell structure control agent and 15 parts of a diluent; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method; the surfactant is diethanolamide stearic acid monoglyceride; the first stabilizer comprises 50wt% of Ba/Zn complex stabilizer and 26wt% of polyether triol and 24wt% of polyoxyethylene-polyoxypropylene copolymer; the resin is polystyrene; the second stabilizer comprises 58wt% of tert-butyl 2-ethylhexoate peroxide and 42wt% of calcium ricinoleate; the foam structure control agent is zirconium phosphate; the diluent is methyl ethyl ketone;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 100 ℃, the curing reaction time is 10h, filtering, washing and drying are carried out, the drying temperature is 70 ℃, and the drying time is 18h, so that the flexible pore material is finally obtained.
Comparative example 5
A method of preparing a flexible pore material, wherein: the method comprises the following steps:
s1, adding 6 parts of surfactant and 3 parts of first stabilizer into 40 parts of deionized water to prepare a homogeneous aqueous solution serving as a water phase; preparing 20 parts of resin, 3 parts of second stabilizer, 5 parts of cell structure control agent, 4 parts of accelerator and 20 parts of diluent into a homogeneous oil solution serving as an oil phase; rapidly mixing the water phase and the oil phase, and preparing an emulsion by a homogenizing emulsification, stirring or ultrasonic method; the surfactant is cocoyl diethanolamide, the first stabilizer comprises 55wt% of a Ba/Zn composite stabilizer and 30wt% of polyether triol and 15wt% of polyoxyethylene-polyoxypropylene copolymer, the resin is polyethylene, the second stabilizer comprises 60wt% of tert-butyl 2-ethyl hexanoate peroxide and 40wt% of calcium ricinoleate, the cell structure controlling agent is zinc carbonate, the accelerator is graphene oxide, and the diluent is isopropanol;
s2, polymerizing the prepared emulsion, wherein the polymerization temperature is 120 ℃, the curing reaction time is 8h, filtering, washing and drying are carried out, the drying temperature is 80 ℃, and the drying time is 15h, so that the flexible porous material is finally obtained.
The results of the performance tests of examples 1 to 3 and comparative examples 1 to 5 are shown below, and the results are shown in Table 1
TABLE 1
Comparing examples 1-3 with comparative examples 1-5, it can be seen that the foamed microporous material prepared by the preparation method of the invention has the advantages of controllable average particle size, regular cellular structure, good compression resilience, good flexibility and excellent stability.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. A preparation method of a flexible porous material is characterized by comprising the following steps: the method comprises the following steps:
s1, adding 2-6 parts of surfactant and 1-3 parts of first stabilizer into 30-40 parts of deionized water to prepare homogeneous aqueous solution serving as a water phase; preparing 5-20 parts of resin, 4-7 parts of propylene-styrene-butadiene copolymer, 1-3 parts of second stabilizer, 3-5 parts of cell structure control agent, 1-4 parts of accelerant and 10-20 parts of diluent into homogeneous oil solution serving as an oil phase; rapidly mixing the water phase and the oil phase, and then preparing an emulsion by a homogeneous emulsification, stirring or ultrasonic method, wherein the first stabilizer comprises 40-55wt% of Ba/Zn composite stabilizer, 25-30 wt% of polyether triol and 15-35 wt% of polyoxyethylene-polyoxypropylene copolymer, and the second stabilizer comprises 55-60 wt% of tert-butyl 2-ethyl hexanoate peroxide and 40-45 wt% of calcium ricinoleate;
and S2, polymerizing the prepared emulsion, and filtering, washing and drying to finally obtain the flexible porous material.
2. The method of preparing a flexible porous material according to claim 1, characterized in that: the surfactant of the step S1 is one or more of lauroyl glutamic acid, diethanolamide stearic acid monoglyceride and cocoyl diethanolamide.
3. The method for preparing a flexible porous material according to claim 1, wherein: the resin in the step S1 is one or more of polyurethane, polystyrene, polyvinyl chloride, polyethylene, polypropylene and phenolic resin.
4. The method of preparing a flexible porous material according to claim 1, characterized in that: the step S1 is that the cell structure control agent is one or more of sodium carbonate, barium carbonate, zirconium phosphate and zinc carbonate.
5. The method of preparing a flexible porous material according to claim 1, characterized in that: the step S1 accelerant is graphene oxide.
6. The method for preparing a flexible porous material according to claim 1, wherein: the diluent in the step S1 is one or more of n-hexane, methyl ethyl ketone, acetone or isopropanol.
7. The method for preparing a flexible porous material according to claim 1, wherein: the polymerization temperature of the step S2 is 60-120 ℃, and the curing reaction time is 8-16h.
8. The method of preparing a flexible porous material according to claim 1, characterized in that: and in the step S2, the drying temperature is 60-80 ℃, and the drying time is 15-20h.
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| CN102417552A (en) * | 2011-09-22 | 2012-04-18 | 中国科学院过程工程研究所 | Polymer nanomicrosphere product with uniform and controllable size and preparation method thereof |
| CN110305483A (en) * | 2019-07-02 | 2019-10-08 | 陕西师范大学 | A kind of low density porous polymer material of flexibility, preparation method and its application as physical protection material |
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| CN110305483A (en) * | 2019-07-02 | 2019-10-08 | 陕西师范大学 | A kind of low density porous polymer material of flexibility, preparation method and its application as physical protection material |
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