CN103865186B - Microemulsion composite of polyethylene wax oxide and preparation method thereof - Google Patents
Microemulsion composite of polyethylene wax oxide and preparation method thereof Download PDFInfo
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- CN103865186B CN103865186B CN201210536545.5A CN201210536545A CN103865186B CN 103865186 B CN103865186 B CN 103865186B CN 201210536545 A CN201210536545 A CN 201210536545A CN 103865186 B CN103865186 B CN 103865186B
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- -1 polyethylene Polymers 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920000573 polyethylene Polymers 0.000 title abstract description 8
- 239000004698 Polyethylene Substances 0.000 title abstract description 7
- 239000002131 composite material Substances 0.000 title abstract description 4
- 239000004530 micro-emulsion Substances 0.000 title abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000007908 nanoemulsion Substances 0.000 claims abstract description 25
- 241000153282 Theope Species 0.000 claims abstract description 12
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 10
- 239000007957 coemulsifier Substances 0.000 claims abstract description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 27
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 15
- 150000005846 sugar alcohols Polymers 0.000 claims description 9
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- NNJVILVZKWQKPM-UHFFFAOYSA-N Lidocaine Chemical compound CCN(CC)CC(=O)NC1=C(C)C=CC=C1C NNJVILVZKWQKPM-UHFFFAOYSA-N 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 229960004194 lidocaine Drugs 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N n-Butanol Substances CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- RPPCFYFWGVIQFS-UHFFFAOYSA-N 1-(dimethylamino)butan-1-ol Chemical compound CCCC(O)N(C)C RPPCFYFWGVIQFS-UHFFFAOYSA-N 0.000 claims description 2
- BFSVOASYOCHEOV-UHFFFAOYSA-N 2-diethylaminoethanol Chemical compound CCN(CC)CCO BFSVOASYOCHEOV-UHFFFAOYSA-N 0.000 claims description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229960002887 deanol Drugs 0.000 claims description 2
- 239000003995 emulsifying agent Substances 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- AYRBHTOSHJHALD-UHFFFAOYSA-N 1-amino-2-methylpropan-1-ol Chemical compound CC(C)C(N)O AYRBHTOSHJHALD-UHFFFAOYSA-N 0.000 claims 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims 1
- BQODPTQLXVVEJG-UHFFFAOYSA-N [O].C=C Chemical group [O].C=C BQODPTQLXVVEJG-UHFFFAOYSA-N 0.000 claims 1
- 239000000839 emulsion Substances 0.000 abstract description 24
- 238000004945 emulsification Methods 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 7
- 239000008187 granular material Substances 0.000 abstract description 5
- 239000004209 oxidized polyethylene wax Substances 0.000 description 32
- 235000013873 oxidized polyethylene wax Nutrition 0.000 description 32
- 239000001993 wax Substances 0.000 description 19
- 239000003153 chemical reaction reagent Substances 0.000 description 12
- 230000001804 emulsifying effect Effects 0.000 description 12
- 229940126680 traditional chinese medicines Drugs 0.000 description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 7
- 239000004094 surface-active agent Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 description 2
- 239000003077 lignite Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000008387 emulsifying waxe Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
Classifications
-
- 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
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/30—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by oxidation
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/05—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- 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
- 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
- C08J2323/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
- C08J2323/30—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by oxidation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/54—Aqueous solutions or dispersions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention discloses a kind of microemulsion composite of polyethylene wax oxide and preparation method thereof.This emulsion compositions contains: 1) 15 35 weight % fusing points are the OPE of 110 150 DEG C, 2) 3 15 weight % nonionic surfactant, 3) 0.5 5 weight % organic alcohol amine co-emulsifier, with 4) 50 80 weight % water, on the basis of the gross weight of described OPE nano-emulsion composition.This emulsion compositions can be prepared with multistep high temperature emulsion process.This wax emulsion particle diameter is less than 100nm and is evenly distributed, dewatering ability, acid and alkali-resistance good stability, and the cold water of available arbitrary proportion dilutes and separates out without granule, and storage stability was more than 6 months.
Description
Technical field
The present invention relates to microemulsion composite of polyethylene wax oxide and preparation method thereof, be particularly used for spinning
High-melting-point OPE nano-emulsion composition knitting industry and preparation method thereof.
Background technology
OPE (Oxidized polyethylene wax)) it is the oxidation of low molecular weight polyethylene
Product.The cere glossiness that oxidized polyethylene wax emulsion is formed is high, and hardness is big, and good hand touch, having can
Polishability, self-repairability, anti-scratch and ruggedness, be widely used in leather, papermaking, weaving etc.
Field.The OPE that field of textiles uses is generally based on emulsion state.Can be as on yarn
Slurry agent, improves flexibility and the lubricity of fiber.Wax emulsion is added in noniron finish working solution, can
To improve tearing brute force and the wearability of fabric.Cotton knitwear is arranged by wax emulsion, it is possible to decrease
The coefficient of friction of yam surface, reduces fluffing probability, thus substantially increases the anti-fluffing and anti-pilling of fabric
Performance.Wax emulsion can be used for soft finish and the water repellent finish etc. of fabric.
Fusing point high point according to OPE uses different emulsification methods, and emulsification method generally may be used
It is divided into normal pressure emulsion process and high-pressure emulsification method.Normal pressure emulsion process is suitable for emulsifying low melting point oxidic polyethylene
Wax, the high-pressure emulsification method emulsifying fusing point OPE more than 105 DEG C is with the obvious advantage.Low melting point oxygen
Change and domestic have a lot of patents and document to report prepare of polythene wax emulsion.As CN101289540A,
CN102206350A, CN102190801A, CN102030996A, CN101503519A etc. are special
Profit.Although CN101289540A, CN102206350A, CN102190801A use high pressure
Emulsion process, but emulsifying is for Honeywell company specific low melting point OPE
AC-629, its fusing point is 101 DEG C.
At present high-melting-point oxidized polyethylene wax emulsion be mainly some multinational giants such as BASF, Clariant,
CHT, Honeywell are selling.Patent CN102532919A report a kind of nanometer paraffin wax emulsion and
Its preparation method, the wax good emulsion stability of preparation, narrow diameter distribution.Although the fusing point of Tissuemat E
Reach 105-120 DEG C, but in order to reduce emulsifying difficulty, emulsion process has added the brown coal of 5-40%
Wax, lignite wax is low melt wax, and fusing point is between 75～86 DEG C.CN102532919A is actually
The mixture of emulsifying high-melting-point and low melt wax, is not the single high-melting-point oxidic polyethylene of emulsifying
Wax.With regard to known to present inventor, the domestic emulsifying to single high-melting-point OPE rarely has document
Research, patent is the most rare.
Therefore, the preparation method of research invention high-melting-point OPE nanoemulsions, have the heaviest
The practical value wanted and realistic meaning.
Summary of the invention:
It is an object of the invention to provide a kind of high-melting-point OPE nano-emulsion composition and
Its preparation method.
The OPE nano-emulsion composition of the present invention contains: 1) 15-35 weight % fusing point is
The OPE of 110-150 DEG C, 2) 3-15 weight % nonionic surfactant, 3) 0.5-5
Weight % organic alcohol amine co-emulsifier, and 4) 50-80 weight % water, receive with described OPE
On the basis of the gross weight of rice emulsion compositions.
The preparation method of OPE nano-emulsion composition of the present invention comprises the following steps:
(1) by OPE that fusing point is 110-150 DEG C, nonionic surfactant, organic
Hydramine co-emulsifier and account for total Water 25-55 weight % Part I water add autoclave, seal,
Stirring；(2) it is warming up to 135-165 DEG C, this temperature range inside holding 20-90 minute；(3) to height
Pressure still adds the Part II water accounting for total Water 45-75 weight % being heated to 95-100 DEG C,
135-165 DEG C is continued insulation 10-30 minute；(4) it is quickly cooled to room temperature, filters, discharging,
Obtain OPE nano-emulsion composition.
This invention use high-pressure emulsification method, the wax emulsion particle diameter of preparation be less than 100nm, size tunable,
It is evenly distributed, dewatering ability, acid and alkali-resistance good stability, store more than 6 months.Use is not had to contain
The emulsifying agent of APEO, is the product of a kind of environmental protection.
Accompanying drawing explanation
Fig. 1 is the grading curve of the oxidized polyethylene wax emulsion that embodiment 1 obtains.
Fig. 2 is the grading curve of the oxidized polyethylene wax emulsion that embodiment 2 obtains.
Fig. 3 is the grading curve of the oxidized polyethylene wax emulsion that embodiment 3 obtains.
Detailed description of the invention:
In one preferred embodiment, the OPE nano-emulsion composition of the present invention contains
Have:
1) 20-32 weight % fusing point is the OPE of 120-140 DEG C,
2) 5-10 weight % nonionic surfactant,
3) 0.5-3 weight % organic alcohol amine co-emulsifier, and
4) 55-70 weight % water, with the gross weight of described OPE nano-emulsion composition be
Benchmark.
The height of fusing point determines the selection of emulsifying OPE method, also reflects the difficulty of emulsifying
Easily degree.Although not having science to define and strict boundary high-melting-point and low melting point OPE
Limit, for purposes of the present invention, high-melting-point OPE of the present invention refers to that fusing point is the highest
In the OPE of 120 DEG C.
In one preferred embodiment, above-mentioned nonionic surfactant includes fatty alcohol polyoxy
Vinyl Ether, aliphatic amine polyoxyethylene ether, polyhydric alcohol polyoxyethylene ether or combinations thereof thing.
In a preferred embodiment, above-mentioned fatty alcohol-polyoxyethylene ether has following knot
Structure:
CxH2x+1O(CH2CH2O)yH, x=10-18, y=4-16；
Described aliphatic amine polyoxyethylene ether has a following structure:
CnH2n+1N(CH2CH2O)mH(CH2CH2O)pH, n=12-18, m+p=5-20；
Described polyhydric alcohol polyoxyethylene ether is glycerin polyoxyethylene ether (10-20) and Pehanorm
Polyoxyethylene ether (12-20).
In a preferred embodiment, above-mentioned fatty alcohol-polyoxyethylene ether, fatty amine polyoxy
Vinyl Ether, the weight ratio of polyhydric alcohol polyoxyethylene ether be: fatty alcohol-polyoxyethylene ether 30-80 weight %,
Aliphatic amine polyoxyethylene ether 20-70% weight, polyhydric alcohol polyoxyethylene 5-30 weight %, in described
On the basis of the gross weight of property surfactant.
In a preferred embodiment, above-mentioned organic alcohol amine co-emulsifier includes dimethylamino
Ethanol, diethylaminoethanol, lignocaine propanol, dimethylamino butanol, 5-lignocaine-2-amylalcohol；
In 2-ethylamino-n-butyl alcohol, 2-amino-1-amylalcohol, 5-amino-1-amylalcohol, 2-amino-2-methyl-propanol
One or both.
In one preferred embodiment, the present invention uses deionized water.
In one preferred embodiment, the OPE nano-emulsion composition of the present invention is also
Alkali metal hydroxide, alkali metal pyrosulfite or their mixture containing 0.2-5 weight.
In a preferred embodiment, the OPE nano-emulsion composition of the present invention contains
Potassium hydroxide 0.2-3%, sodium sulfite 0.2-1% or their mixture.
The OPE nano-emulsion composition of the present invention can be by the method system comprised the steps
Standby:
(1) by OPE that fusing point is 110-150 DEG C, nonionic surfactant, organic
Hydramine co-emulsifier, account for total Water 30-55 weight % Part I water add autoclave, seal,
Stirring；
(2) it is warming up to 135-165 DEG C, this temperature range inside holding 20-90 minute；
(3) add in autoclave be heated to 95-100 DEG C account for the of total Water 45-70 weight %
Two part water, continue insulation 10-30 minute at 135-165 DEG C；
(4) it is quickly cooled to room temperature, filters, discharging, obtain OPE nanoemulsions group
Compound.
In one preferred embodiment, the 1st step adds alkali metal hydroxide, alkali metal
Pyrosulfite or their mixture, to regulate the pH of OPE nano-emulsion composition
Value and some impurity removed in raw material.The pH of OPE nano-emulsion composition of the present invention
Value generally alkalescence, preferably pH 8-12, preferably 8.5-10.5.
If it is desired, the 3rd step in the inventive method can point multistep be carried out, generally 2-4 walks,
But preferably 1 step is carried out.
Oxidized polyethylene wax emulsion prepared by the present invention, particle diameter is less than 100nm, is evenly distributed, centrifugal
Stability, acid and alkali-resistance good stability, store more than 6 months performances still stable.
Embodiment
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are only used
In the explanation present invention rather than restriction the scope of the present invention.In addition, it is to be understood that reading the present invention
After the content lectured, the present invention can be made various changes or modifications by those skilled in the art, these
The equivalent form of value falls within the application appended claims limited range equally.
Experimental data in each embodiment measures according to following method:
Dewatering ability measures: use medical centrifuge (TDZ5-WS) under the rotating speed of 3000rpm
Centrifugal 30 minutes, see whether to occur floating, be layered, precipitate.
Particle size determination: the wax emulsion solution of preparation 1%, with Zetasizer Nano S90(Malvern
Company) nano particle size instrument measures its mean diameter and polydispersity index PDI.Polydispersity index is the least,
Particle diameter distribution is the most uniform.
Acid and alkali-resistance stability: the wax emulsion of preparation is regulated pH to 2 and 12 with acetic acid and liquid caustic soda respectively,
See whether that layering and precipitation occur.
Dilution stability: by the deionized water dilution of the wax emulsion arbitrary proportion of preparation, see whether
Little granule is had to separate out.
Embodiment 1
By 220g OPE Luwax OA6(BASF, fusing point 126-133 DEG C), 24gAEO-9
(SINO SURFACTANT), 18g AC-1215(Jiangsu Hai'an Petrochemical Plant), 4g sweet
Oil polyoxyethylene ether (SINO SURFACTANT), 5g potassium hydroxide (traditional Chinese medicines reagent), 2g are burnt
Sodium sulfite (traditional Chinese medicines reagent), 4g 5-lignocaine-2-amylalcohol (traditional Chinese medicines reagent), 8g 5-amino-1-
Amylalcohol (traditional Chinese medicines reagent) and 208g deionized water add 1 liter of high pressure emulsifying kettle (CJF-1, Shanghai assistant officer
Bright instrument and equipment company limited), seal, start stirring (500 revs/min).It is warming up to 150 DEG C, protects
Temperature 30 minutes.Then in emulsifying kettle, add the deionized water 230g of 95-100 DEG C, continue at 150 DEG C
Continuation of insurance temperature 30 minutes.It is quickly cooled to room temperature, filters, discharging, obtain faint yellow translucent oxidation
Tissuemat E nanoemulsions.
With Zetasizer Nano S90 nano particle size instrument, gained wax emulsion is measured, as it is shown in figure 1,
Mean diameter is 46.89nm, and polydispersity index is 0.208, even particle size distribution.Test by centrifugation,
Without floating, without layering, without precipitation.Through acid and alkali-resistance stability test, in the range of pH 2-12, nothing
Layering, nothing precipitation.Arbitrarily dilute through deionized water, separate out without granule.
Embodiment 2
By 180g OPE Licowax PED 191(Clariant, fusing point 123 DEG C), 24g
Paregal O-15(Jiangsu Hai'an Petrochemical Plant), 24gAC-1210(Jiangsu Province Hai'an oil
Factory), 2g trimethylolpropane polyoxyethylene ether (SINO SURFACTANT), 7g hydroxide
Potassium (traditional Chinese medicines reagent), 1.8g sodium pyrosulfite (traditional Chinese medicines reagent), 2g lignocaine propanol (traditional Chinese medicines
Reagent), 12g 2-amino-2-methyl-propanol (traditional Chinese medicines reagent) and 180g deionized water add 1 liter
High-pressure emulsification still (CJF-1, Shanghai Cheng Ming instrument and equipment company limited), seals, and starts stirring (500
Rev/min).It is warming up to 135 DEG C, is incubated 60 minutes.Then in emulsifying kettle, add 95-100 DEG C go
Ionized water 280g, continues insulation 20 minutes at 135 DEG C.It is quickly cooled to room temperature, filters, discharging,
Obtain milky translucent OPE nanoemulsions.
With Zetasizer Nano S90 nano particle size instrument, gained wax emulsion is measured, as in figure 2 it is shown,
Mean diameter is 31.96nm, and polydispersity index is 0.157, even particle size distribution.Test by centrifugation,
Without floating, without layering, without precipitation.Through acid and alkali-resistance stability test, in the range of pH 2-12, nothing
Layering, nothing precipitation.Arbitrarily dilute through deionized water, separate out without granule.
Embodiment 3
By 150g OPE AC-330(Honeywell, fusing point 137 DEG C), 20g 1310
(Jiangsu Hai'an Petrochemical Plant), 20g AC-1812(Jiangsu Hai'an Petrochemical Plant), 10g
Glycerin polyoxyethylene ether (SINO SURFACTANT), 10g potassium hydroxide (traditional Chinese medicines reagent), 5g
Sodium pyrosulfite (traditional Chinese medicines reagent), 4g 2-ethylamino-n-butyl alcohol (traditional Chinese medicines reagent), 16g 5-amino-1-
Amylalcohol (traditional Chinese medicines reagent) and 160g deionized water add high-pressure emulsification still (CJF-1, the bright instrument of Shanghai assistant officer
Device equipment company limited), seal, start stirring (500 revs/min).It is warming up to 160 DEG C, is incubated 60
Minute.Then in emulsifying kettle, add the deionized water 320g of 95-100 DEG C, continue insulation at 160 DEG C
30 minutes.It is quickly cooled to room temperature, filters, discharging, obtain the translucent OPE of milky
Nanoemulsions.
With Zetasizer Nano S90 nano particle size instrument, gained wax emulsion is measured, as it is shown on figure 3,
Mean diameter is 55.10nm, and polydispersity index is 0.191, even particle size distribution.Test by centrifugation,
Without floating, without layering, without precipitation.Through acid and alkali-resistance stability test, in the range of pH 2-12, nothing
Layering, nothing precipitation.Arbitrarily dilute through deionized water, separate out without granule.
Claims (9)
1. the preparation method of OPE nano-emulsion composition, described OPE
Nano-emulsion composition, it is made up of following component:
1) 15-35 weight % fusing point is the OPE of 120-150 DEG C,
2) 5-15 weight % nonionic surfactant,
3) 0.5-5 weight % organic alcohol amine co-emulsifier, and
4) 50-80 weight % water, with the gross weight of described OPE nano-emulsion composition be
Benchmark, and the percetage by weight summation of each component is 100%；
It is characterized in that this preparation method comprises the following steps:
(1) by OPE, nonionic surfactant, organic alcohol amine co-emulsifier, account for
The Part I water of total Water 25-55 weight % adds autoclave, seals, stirring；
(2) it is warming up to 135-165 DEG C, this temperature range inside holding 20-90 minute；
(3) add in autoclave be heated to 95-100 DEG C account for the of total Water 45-75 weight %
Two part water, continue insulation 10-30 minute at 135-165 DEG C；
(4) it is quickly cooled to room temperature, filters, discharging, obtain OPE nanoemulsions group
Compound.
2. the preparation method of OPE nano-emulsion composition as claimed in claim 1,
It is characterized in that: in the 1st step add alkali metal hydroxide, alkali metal pyrosulfite or they
Mixture.
3. the preparation method of OPE nano-emulsion composition as claimed in claim 1,
It is characterized in that: the 3rd step can divide 2-4 step to carry out.
4. the method for claim 1, it is characterised in that it is made up of following component:
1) 20-32 weight % fusing point is the OPE of 120-140 DEG C,
2) 5-10 weight % nonionic surfactant,
3) 1-3 weight % organic alcohol amine co-emulsifier, and
4) 55-70 weight % water, with the gross weight of described OPE nano-emulsion composition be
Benchmark.
5. the method as described in claim 1 or 4, it is characterised in that described non-ionic surface is lived
Property agent include fatty alcohol-polyoxyethylene ether, aliphatic amine polyoxyethylene ether, polyhydric alcohol polyoxyethylene ether or
Combinations thereof thing.
6. method as claimed in claim 5, it is characterised in that described fatty alcohol-polyoxyethylene ether
There is following structure:
CxH2x+1O(CH2CH2O)yH, x=10-18, y=4-16；
Described aliphatic amine polyoxyethylene ether has a following structure:
CnH2n+1N(CH2CH2O)mH(CH2CH2O)pH, n=12-18, m+p=5-20；
Described polyhydric alcohol polyoxyethylene ether is glycerin polyoxyethylene ether 10-20 and Pehanorm gathers
Oxygen vinyl Ether 12-20.
7. method as claimed in claim 5, it is characterised in that it is characterized in that: described fat
Fat polyoxyethylenated alcohol, aliphatic amine polyoxyethylene ether, the weight ratio of polyhydric alcohol polyoxyethylene ether be: fat
Fat polyoxyethylenated alcohol 30-80 weight %, aliphatic amine polyoxyethylene ether 20-70% weight, polyhydric alcohol gathers
Oxygen ethylene 5-30 weight %, on the basis of the gross weight of described nonionic surfactant, and fatty alcohol
Polyoxyethylene ether, aliphatic amine polyoxyethylene ether, the percetage by weight summation of polyhydric alcohol polyoxyethylene ether are
100%.
8. the method as described in claim 1 or 4, it is characterised in that: described organic alcohol amine helps
Emulsifying agent include dimethylaminoethanol, diethylaminoethanol, lignocaine propanol, dimethylamino butanol,
5-lignocaine-2-amylalcohol；2-ethylamino-n-butyl alcohol, 2-amino-1-amylalcohol, 5-amino-1-amylalcohol, 2-
One or both in amino-2-methyl-propanol.
9. the method as described in claim 1 or 4, it is characterised in that it is possibly together with 0.2-5 weight %
Alkali metal hydroxide, alkali metal pyrosulfite or their mixture, described water be from
Sub-water.
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| CN113121844A (en) * | 2019-12-31 | 2021-07-16 | 广州麦吉高分子新材料科技有限公司 | Preparation method of nanoscale emulsified wax |
| CN111234261A (en) * | 2020-03-26 | 2020-06-05 | 湖南科技大学 | Two-step emulsification method for preparing high-density oxidized polyethylene microemulsion |
| CN111234260A (en) * | 2020-03-27 | 2020-06-05 | 东莞市汉维科技股份有限公司 | Two-step emulsification preparation process of super-hydrophobic paraffin/polyethylene wax composite microemulsion |
| CN111253589A (en) * | 2020-03-27 | 2020-06-09 | 东莞市汉维科技股份有限公司 | Two-step emulsification preparation process of super-hydrophobic high-density oxidized polyethylene microemulsion |
| CN111393674B (en) * | 2020-05-13 | 2023-07-18 | 宁波德曜新材料有限公司 | Aqueous oxidized polyethylene wax emulsion and preparation method thereof |
| CN114369257A (en) * | 2022-01-26 | 2022-04-19 | 襄阳市岩翔化工有限公司 | High-melting-point wax emulsion for papermaking and preparation method thereof |
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