CN105111588B - A kind of intelligent thermoregulating master batch and preparation method thereof - Google Patents
A kind of intelligent thermoregulating master batch and preparation method thereof Download PDFInfo
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- CN105111588B CN105111588B CN201510611679.2A CN201510611679A CN105111588B CN 105111588 B CN105111588 B CN 105111588B CN 201510611679 A CN201510611679 A CN 201510611679A CN 105111588 B CN105111588 B CN 105111588B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention provides a kind of intelligent thermoregulating master batch and preparation method thereof, the phase-change microcapsule containing surface hydrophobicity in master batch.Common microcapsule surface hydrophilic, in the techniques such as granulation, spinning, the poor compatibility with polymeric substrate.Not only cause master batch hydraulic performance decline, and microcapsules waste is very big.Phase-change microcapsule surface hydrophobicity in technical solution of the present invention, fine heat-resisting performance good with polymeric matrix compatible.Extensively, manufacture method is workable, and cost is low, beneficial to popularization for the optional polymeric substrate species of this method.Intelligent thermoregulating master batch of the present invention is used for melt spinning, non-woven fabrics and thin film fabrication, the field such as plastic-injection shaping, has positive role to providing product quality and the market competitiveness.
Description
Technical field
The present invention relates to a kind of feature agglomerate material, and in particular to a kind of intelligent thermoregulating master batch and preparation method thereof.
Background technology
Master batch is a kind of important polymer intermediate products, to be convenient to transport, store and machine-shaping.The purposes of master batch
It is quite varied, the various plastic tubs in such as daily life, bucket, film；It is used to manufacture non-woven fabrics, fiber, footwear in textile industry
Material etc.；It is used to produce various pipelines, plastic door-window etc. in construction material；Or even mechanical industry, aerospace industry, agricultural production etc.
Various comprehensive products.
For numerous products, the function of master batch is very crucial.Intelligent thermoregulating functional product, such as temperature-regulating fiber, temperature-regualting base
Chair etc., is the new product that the state such as America and Europe rises in recent years.China rises year by year to the import volume of such intelligent thermoregulating functional product,
But it is domestic still without formation large-scale production.
Intelligent thermoregulating function is that, by adding phase-change material, often the phase-change microcapsule of micro/nano level is realized.By
There is phase-state change process release simultaneously at a certain temperature or the characteristic of absorption heat in phase-change material, with heating/drop
Warm bidirectional modulation temperature function, thus it is referred to as intelligent thermoregulating material.As outlast companies of the U.S. are molten using phase-change microcapsule
Liquid, has been made the fibers such as acrylic fibers, viscose, but this method is only suitable for wet spinning technology.Melt-spinning technology has a variety of limitations.
And in melt-spinning technology, master batch or the manufacturing process for being called spinning master batch, and subsequent melt spinning
Process, temperature is typically at 200 DEG C -300 DEG C.Phase-change microcapsule shell material prepared by conventional method can not often bear so harsh
Processing conditions, even if completing spinning reluctantly, the loss of phase-change material also can be very big, directly contributes the rise of manufacturing cost, and
Cause the unstable of technique.
Application for a patent for invention number 200810157553.2, describes a kind of phase-change material micro-capsule preparation side of high temperature resistant type
Method, by introducing phenyl ring in the shell material of phase-change microcapsule, improves the heat resisting temperature upper limit of phase-change microcapsule.But this method
Microcapsules shell material be modified melamine formaldehyde resin, with being hydrophily shell traditional most of microcapsules shell materials
Material.In spinning technique, the raw material of master batch, such as polyester, polypropylene are hydrophobic material.Therefore in spinning process, deposit
The problem of phase-change microcapsule is incompatible with matrix material.This is resulted in the blending and spinning process of material, the micro- glue of phase transformation
Capsule is easily separated with master batch base material, or even can not mix completely.Directly the problem of be exactly, the phase transformation in master batch
Microencapsulation material content is very low, or phase-change microcapsule is only distributed only over the surface of master batch, is easily lost in secondary operation.
Inventors noted that if the phase-change microcapsule content carried out with above-mentioned master batch in spinning, gained fiber is inevitable
It is very limited, it is contemplated that feature be even more not know that where to talk.
To solve consistency problem, application for a patent for invention number 201010284818.2 provides a kind of in polyurethane resin conjunction
Into middle addition polyethylene glycol etc. as soft segment, then the method for carrying out polymerisation in bulk, the resin of gained can carry out spinning granulation.The party
Method solves consistency problem by the formation of chemical bond, but the key of method is the formation of chemical bond, and this is enabled to
The material of application is very limited.Meanwhile, the result of chemical reaction result in the phase transition temperature of phase-change material, phase transformation enthalpy all by
Considerable influence.It directly results in the change of master batch quality.Although solving consistency problem, but introduce female to polymer
The larger new problem of grain influence.
As can be seen here, a kind of and excellent intelligent thermoregulating functional agglomerate preparation method of substrate compatibility is found with very heavy
The realistic meaning wanted.
The content of the invention
This method discloses a kind of intelligent thermoregulating master batch, and it has intelligent thermoregulating function, and by being dredged in master batch containing surface
Aqueous phase-change microcapsule is realized.The preparation method of the intelligent thermoregulating master batch of the present invention includes step：
(1) surface hydrophobicity phase-change microcapsule is prepared；
(2) master batch is made in the phase-change microcapsule of above-mentioned surface hydrophobicity and polymeric substrate blending；
Produce described intelligent thermoregulating master batch.
The phase-change microcapsule preparation method of wherein described surface hydrophobicity includes：1) in the organic solvent containing surfactant
In, phase-change material, and shell material monomer solution are added, reversed-phase emulsion is formed；2) after heating response, isolated surface hydrophobicity
Phase-change microcapsule.
The surfactant, including nonionic surfactant；
One kind in the organic solvent, including petroleum ether, n-hexane, hexamethylene, atoleine, toluene or dimethylbenzene or
Several combinations；
The phase-change material, including at least one of alkali metal salt, alkali salt, polyethylene glycol or its aqueous solution.
The shell material monomer solution, includes the aqueous solution of at least one of phenols, aldehydes, amine.
In the method for preparing surface hydrophobicity phase-change microcapsule, the Adding Way of aqueous phase, including once add and in batches
Add.
The polymeric substrate, including polyethylene, polytetrafluoroethylene (PTFE), polyvinyl chloride, polyethylene, polypropylene, polystyrene,
Polymethyl methacrylate, polyethylene terephthalate, PTT, polybutylene terephthalate
At least one of ester, makrolon, polyamide, polyurethane, EVA, PLA, TPE, ABS or its spread out
It is biological.
The phase-change microcapsule prepared by methods described, because course of reaction is entered in the reversed-phase emulsion of water-in-oil type
OK, shell material is when oil-water interfaces are formed, and hydrophobic parts are more likely to oil phase, therefore form hydrophobic phase-change microcapsule.
Microcapsule wall material after the completion of reaction, main component is various types of phenolic resin.Phenolic resin excellent heat resistance, completely may be used
Processing and follow-up technological requirement are manufactured with the master batch for bearing 200-300 DEG C.
Common microcapsule surface hydrophilic, in the techniques such as granulation, spinning, the poor compatibility with polymeric substrate.Not only lead
Master batch hydraulic performance decline is caused, and microcapsules waste is very big.Phase-change microcapsule surface hydrophobicity in technical solution of the present invention, with
Polymeric matrix compatible is good, fine heat-resisting performance.The optional polymeric substrate species of this method is extensive, manufacture method operability
By force, cost is low, beneficial to popularization.Intelligent thermoregulating master batch of the present invention be used for melt spinning, non-woven fabrics and thin film fabrication, plastic-injection into
, there is positive role in the fields such as type to providing product quality and the market competitiveness.
Using the beneficial effect of the present invention program：
1) compared to traditional handicraft, the invention provides a kind of preparation method of feature master batch；
2) in spinning field, the inventive method is more applicable for melt spinning；
3) in compatibility, compared to methods such as chemical graft, modifications, the applicable polymerizable material species of the present invention is more
It is many, while to the property such as phase transition temperature of phase-change material, the influence of phase transformation enthalpy is small；
4) more preferably, master batch processing and subsequent machining technology loss are small for the microcapsule wall material heat resistance in the inventive method；
5) cost is low, it is easy to promote.
The intelligent thermoregulating master batch that the present invention is provided, application field includes：Melt spinning and thin film fabrication, plastic-injection into
Type.
Brief description of the drawings
Fig. 1 is that the master batch DSC prepared by the embodiment of the present invention characterizes curve.
Embodiment
The present invention is specifically addressed below by embodiment.
Embodiment 1：
1. prepare the phase-change microcapsule of surface hydrophobicity
10g Span-80 formation oil-phase solutions A is added in 100ml hexamethylenes；
3g resorcinols and 5g acetaldehyde formation aqueous phase solution B are added in 5g deionized waters；
It is added to after solution B and 5g cetomacrogol 1000s are well mixed in solution A, stirring forms inverse emulsion C；
2g aniline solutions are added dropwise into emulsion C, 50 DEG C are heated to, 30min is reacted；
Filtered after reaction, wash, separate, dry, form a kind of phase transformation of the surface hydrophobicity of benzoxazine colophony cladding micro-
Capsule.
2. by surface hydrophobicity phase-change microcapsule and polypropylene described in 1, with mass ratio 40：60, at 160-200 DEG C with double
Screw extruder blending granulation；
Obtain intelligent thermoregulating polypropylene agglomerate of the present invention.After testing, obtained master batch DSC characterizes curve such as
Described in Fig. 1.
The master batch passes through further melt spinning, obtains a kind of intelligent thermoregulating polyester fiber.
Embodiment 2
1. prepare surface hydrophobicity phase-change microcapsule：
5g surfactants Span-80 formation oil-phase solutions A is added in 90ml atoleines；
3g anhydrous calcium chlorides are added in 7g deionized waters, aqueous phase solution B is formed；
5g phenol and 6g acetaldehyde formation aqueous phase solution C are added in 6g deionized waters,
Solution B and C are slowly added into solution A, stirring forms stable w/o type emulsion, are heated to 65 DEG C, reaction
4h；Filtering, separation obtains surface hydrophobicity phase-change microcapsule after drying；
2. by surface hydrophobicity phase-change microcapsule and polybutylene terephthalate described in 1, with mass ratio 30：70,
260-300 DEG C is blended granulation with double screw extruder；
Obtain intelligent thermoregulating polyester master particle of the present invention.
The master batch passes through further melt spinning, obtains a kind of intelligent thermoregulating polyester fiber.
Embodiment 3
1. prepare the phase-change microcapsule of surface hydrophobicity：
10g Span-80 formation oil-phase solutions A is added in 80ml n-hexanes；
3g resorcinols and 5g acetaldehyde formation aqueous phase solution B are added in 5g deionized waters；
3g cetomacrogol 1000s and 2g polyethylene glycol 2000s formation aqueous phase solution C are added in 5g deionized waters；
It is added to after solution B and C are well mixed in solution A, stirring forms inverse emulsion D；
2g aniline solutions are added dropwise into emulsion D, 50 DEG C are heated to, 30min is reacted；
Filtered after reaction, washing, separation, a kind of dry, phase-change microcapsule of the surface hydrophobicity of phenolic resin cladding of formation.
2. by the surface hydrophobicity phase-change microcapsule described in 1 and elastic polyurethane body rubber (TPU), with mass ratio 20：80,
It is blended and is granulated with double screw extruder at 130-230 DEG C；
Obtain intelligent thermoregulating TPU master batches of the present invention.
The master batch passes through blown film or calendering technology, obtains a kind of intelligent thermoregulating TPU film.
Embodiment 4
1. prepare the phase-change microcapsule of surface hydrophobicity：
8g Span-80 formation oil-phase solutions A is added in 90ml petroleum ethers；
2g sodium sulphate and 1g cetomacrogol 1000s are added in 5g deionized waters, aqueous phase solution B is formed；
4g phenol and 6g formaldehyde formation aqueous phase solution C are added in 6g deionized waters,
Solution B and C are slowly added into solution A, stirring forms reversed-phase emulsion D；
Filtered after being heated to 70 DEG C, reaction 3.5h, wash, dry, the surface hydrophobicity phase transformation for forming phenolic resin cladding is micro-
Capsule.
2. by surface hydrophobicity phase-change microcapsule and polypropylene described in 1, with mass ratio 40：60, at 160-200 DEG C with double
Screw extruder blending granulation；
Obtain intelligent thermoregulating polypropylene agglomerate of the present invention.
The master batch obtains a kind of intelligent thermoregulating polypropylene fiber through further melt spinning.Or be meltblown master batch, hot rolling
Intelligent thermoregulating non-woven fabrics is made etc. technique.
Embodiment 5
1. prepare the phase-change microcapsule of surface hydrophobicity
10g Span-80 formation oil-phase solutions A is added in 100ml hexamethylenes；
3g resorcinols and 5g acetaldehyde formation aqueous phase solution B are added in 5g deionized waters,
It is added to after solution B and 5g cetomacrogol 1000s are well mixed in solution A, stirring forms inverse emulsion C；
2g aniline solutions are added dropwise into emulsion C, 50 DEG C are heated to, 30min is reacted；
Filtered after reaction, wash, separate, dry, form a kind of phase transformation of the surface hydrophobicity of benzoxazine colophony cladding micro-
Capsule.
2. by the surface hydrophobicity phase-change microcapsule described in 1 and EVA (EVA), with mass ratio 10：
90, it is blended and is granulated with double screw extruder at 140-200 DEG C；
Obtain intelligent thermoregulating EVA master batches of the present invention.
The master batch passes through further injection molding, obtains a kind of intelligent thermoregulating shoe-pad.
Embodiment 6
Step 1,2 is identical with embodiment 4.
By the intelligent thermoregulating polypropylene agglomerate and polybutylene terephthalate of above-mentioned manufacture, with mass ratio 30：70,
260-300 DEG C is blended granulation with double screw extruder；
Obtain intelligent thermoregulating polypropylene/polyester composite master batch of the present invention.
The master batch passes through further melt spinning, obtains a kind of intelligent thermoregulating polypropylene fibre/terylene composite fibre.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, skill of this area ordinary skill technical staff to the present invention
In various modifications and improvement that art scheme is made, the protection domain that claims of the present invention determination all should be fallen into.
Claims (6)
1. a kind of intelligent thermoregulating master batch, it is characterised in that with intelligent thermoregulating function, and by containing surface hydrophobic in master batch
Phase-change microcapsule realize；Its preparation method includes step：
(1) surface hydrophobicity phase-change microcapsule is prepared：Preparation method includes：1) in the organic solvent containing surfactant, plus
Enter phase-change material, and shell material monomer solution, form reversed-phase emulsion；2) after heating response, the phase transformation of isolated surface hydrophobicity
Microcapsules；
(2) intelligent thermoregulating master batch is made in the phase-change microcapsule of above-mentioned surface hydrophobicity and polymeric substrate blending；Wherein described phase
Become at least one of material, including alkali metal salt, alkali salt, polyethylene glycol or its aqueous solution；The shell material monomer water
Solution, includes the aqueous solution of at least one of phenols, aldehydes, amine.
2. intelligent thermoregulating master batch according to claim 1, it is characterised in that the surfactant, including nonionic table
Face activating agent.
3. intelligent thermoregulating master batch according to claim 1, it is characterised in that the organic solvent, including petroleum ether, just oneself
One or more of combinations in alkane, hexamethylene, atoleine, toluene or dimethylbenzene.
4. intelligent thermoregulating master batch according to claim 1, it is characterised in that the surface hydrophobicity phase-change microcapsule for preparing
Method, the Adding Way of aqueous phase, including once add and be added portionwise.
5. intelligent thermoregulating master batch according to claim 1, it is characterised in that the polymeric substrate, including it is polyethylene, poly-
Tetrafluoroethene, polyvinyl chloride, polypropylene, polystyrene, polymethyl methacrylate, polyethylene terephthalate, poly- pair
Benzene dicarboxylic acid trimethylene glycol ester, polybutylene terephthalate (PBT), makrolon, polyamide, polyurethane, polyethylene vinyl acetate
At least one of ester, PLA, TPE, ABS or derivatives thereof.
6. intelligent thermoregulating master batch described in claim any one of 1-5 be applied to melt spinning and thin film fabrication, plastic-injection into
Type.
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Cited By (1)
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| US20220120004A1 (en) * | 2020-10-20 | 2022-04-21 | Shanghai Yongli Transportation System Co., Ltd. | Method for preparing automatic temperature control light conveyor belt |
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| CN110054786A (en) * | 2018-01-18 | 2019-07-26 | 苏州润特新材料科技有限公司 | It is a kind of to improve the method for stable effective ingredients and product preparation in functional master batch |
| CN108822409B (en) * | 2018-07-17 | 2021-05-11 | 佛山市绿盈新材料科技有限公司 | Temperature-adjustable CPP/BOPP composite packaging film and preparation method thereof |
| CN114507906B (en) * | 2022-02-21 | 2023-02-03 | 季华实验室 | Method for preparing polytetrafluoroethylene fiber with storage function by utilizing wet spinning |
| CN117304881A (en) * | 2023-09-26 | 2023-12-29 | 波司登羽绒服装有限公司 | Phase-change microcapsule material and preparation method and application thereof |
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| CN101745352A (en) * | 2009-12-15 | 2010-06-23 | 中国科学院化学研究所 | Superhydrophobic surface material and special nano-particles thereof with core-shell structures |
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| CN102618223A (en) * | 2012-02-27 | 2012-08-01 | 李雨杉 | Phase change material microcapsule coated by thermoset phenolic resin and preparation method thereof |
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| US20220120004A1 (en) * | 2020-10-20 | 2022-04-21 | Shanghai Yongli Transportation System Co., Ltd. | Method for preparing automatic temperature control light conveyor belt |
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