CN116041983A - Surface treatment method of powder for polyurethane heat-conducting pouring sealant - Google Patents
Surface treatment method of powder for polyurethane heat-conducting pouring sealant Download PDFInfo
- Publication number
- CN116041983A CN116041983A CN202211559259.0A CN202211559259A CN116041983A CN 116041983 A CN116041983 A CN 116041983A CN 202211559259 A CN202211559259 A CN 202211559259A CN 116041983 A CN116041983 A CN 116041983A
- Authority
- CN
- China
- Prior art keywords
- powder
- polyurethane
- parts
- pouring sealant
- conducting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 90
- 239000004814 polyurethane Substances 0.000 title claims abstract description 90
- 239000000843 powder Substances 0.000 title claims abstract description 86
- 239000000565 sealant Substances 0.000 title claims abstract description 52
- 238000004381 surface treatment Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 34
- 239000000839 emulsion Substances 0.000 claims abstract description 28
- 150000001450 anions Chemical class 0.000 claims abstract description 13
- 238000001694 spray drying Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229920002521 macromolecule Polymers 0.000 claims abstract description 7
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 4
- 239000007921 spray Substances 0.000 claims abstract description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 26
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 15
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 12
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 9
- 239000004359 castor oil Substances 0.000 claims description 9
- 235000019438 castor oil Nutrition 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- 238000004945 emulsification Methods 0.000 claims description 9
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 9
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 9
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 7
- HPQUMJNDQVOTAZ-UHFFFAOYSA-N 2,2-dihydroxypropanoic acid Chemical compound CC(O)(O)C(O)=O HPQUMJNDQVOTAZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000013530 defoamer Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 150000002513 isocyanates Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000004382 potting Methods 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000000945 filler Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000001282 organosilanes Chemical group 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a surface treatment method of powder for polyurethane heat-conducting pouring sealant, and relates to the technical field of polyurethane heat-conducting pouring sealant; in order to improve the heat conduction effect on the premise of not increasing the viscosity of the system; the method comprises the following steps: preparing carboxylic acid type polyurethane anion emulsion with the molecular structure similar to or the same as that of polyurethane in the polyurethane heat conduction pouring sealant; uniformly mixing the powder to be treated with the polyurethane emulsion according to a certain proportion; spraying the mixture by using a spray dryer to obtain powder with the surface modified by polyurethane macromolecules. According to the invention, polyurethane with a molecular structure similar to or the same as that of polyurethane in the polyurethane heat-conducting pouring sealant is mixed with the heat-conducting powder, and then spray drying is carried out, so that the modified powder with the surface coated with polyurethane macromolecules is obtained, the compatibility of the powder in a polyurethane system is greatly improved, more powder can be filled under the condition of the same viscosity, and the heat-conducting property is improved.
Description
Technical Field
The invention relates to the technical field of polyurethane heat-conducting pouring sealant, in particular to a surface treatment method of powder for polyurethane heat-conducting pouring sealant.
Background
The polyurethane heat conduction pouring sealant is a filling type heat conduction material obtained by adding insulating heat conduction powder such as aluminum hydroxide, aluminum oxide, aluminum nitride, boron nitride and the like into a polyurethane matrix; the material has the characteristics of wide hardness range, chemical corrosion resistance, good elasticity, excellent adhesion and the like of the polyurethane pouring sealant, and also has a heat conduction function; currently, the battery has been widely used in the fields of electronic devices, new energy automobile batteries and the like.
But is limited by the difference between the surface polarity of the heat-conducting powder and the polyurethane system, and the requirement of pouring sealant on the viscosity of the product, the filling amount of the powder is mostly below 90% by weight; the heat conductivity coefficient of the polyurethane heat-conducting pouring sealant sold in the current market is only about 3 w/m.k at most; how to improve the compatibility of the heat conducting filler and a resin system, and increase the addition amount of the heat conducting powder on the premise of not increasing the viscosity of the system, is an urgent problem to be solved for limiting the rapid development of polyurethane heat conducting pouring sealant products.
Through retrieval, the patent with the Chinese patent application number of CN201610831586.5 discloses a heat-conducting pouring sealant and a preparation method thereof, wherein the heat-conducting pouring sealant comprises an agent A and an agent B, the agent A comprises 100 parts by weight of base adhesive, 10-20 parts by weight of heat-conducting filler, 5-7 parts by weight of diluent, 50-60 parts by weight of filler and 1-2 parts by weight of whitening agent, the heat-conducting filler is organosilane and/or titanate surface-treated alumina, and the agent B comprises 7-23 parts by weight of cross-linking agent, 10-20 parts by weight of diluent, 0.5-4 parts by weight of coupling agent and 0.05-0.06 part by weight of catalyst. The heat-conducting pouring sealant in the above patent has the following disadvantages: the compatibility of the heat conducting filler and the resin system is insufficient, the addition amount of the heat conducting material is less, and the heat conducting performance of the final product is also insufficient.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a surface treatment method of powder for polyurethane heat-conducting pouring sealant.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a surface treatment method of powder for polyurethane heat-conducting pouring sealant comprises the following steps:
s1: preparing carboxylic acid type polyurethane anion emulsion with the molecular structure similar to or the same as that of polyurethane in the polyurethane heat conduction pouring sealant;
s2: uniformly mixing the powder to be treated with the polyurethane emulsion according to a certain proportion;
s3: spraying the mixture by using a spray dryer to obtain powder with the surface modified by polyurethane macromolecules.
Preferably: the surface treatment method of the powder specifically comprises the following steps:
s11: adding the raw material A into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s12: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s13: adding triethylamine into the polyurethane prepolymer, and stirring;
s14: stirring, and then pouring into distilled water for emulsification and dispersion;
s15: obtaining polyurethane anion emulsion through reduced pressure distillation;
s16: spherical alumina of D502 microns is mixed with the emulsion according to the mass ratio of 1:2, uniformly mixing;
s17: and (3) spray drying to obtain the alumina powder which can be used in the field of polyurethane heat conduction pouring sealant, wherein the alumina powder is named as powder A.
Further: the surface treatment method of the powder specifically comprises the following steps:
s21: adding the raw material B into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s22: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s23: adding triethylamine into the polyurethane prepolymer, and stirring;
s24: stirring, and then pouring into distilled water for emulsification and dispersion;
s25: obtaining polyurethane anion emulsion through reduced pressure distillation;
s26: d5010 micrometer aluminum hydroxide and the emulsion are mixed according to the mass ratio of 1:2, uniformly mixing;
s27: and (3) spray drying to obtain aluminum hydroxide which can be used in the field of polyurethane heat conduction pouring sealant, wherein the aluminum hydroxide powder is marked as powder B.
Further preferred is: the surface treatment method of the powder specifically comprises the following steps:
s31: adding the raw material C into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s32: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s33: adding triethylamine into the polyurethane prepolymer, and stirring;
s34: stirring, and then pouring into distilled water for emulsification and dispersion;
s35: obtaining polyurethane anion emulsion through reduced pressure distillation;
s36: spherical alumina of D5030 microns is mixed with the emulsion according to the mass ratio of 1:2, uniformly mixing;
s37: and (3) spray drying to obtain the alumina which can be used in the field of polyurethane heat conduction pouring sealant, wherein the alumina powder is named as powder C.
As a preferred embodiment of the present invention: in the step S11, the raw material a includes: 120 parts of liquid polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 4 parts of dimethylol butyric acid, 1.5 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
Further preferred as the present invention is: in the step S21, the raw material B includes: 130 parts of castor oil modified polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 3.5 parts of 2, 2-dihydroxypropionic acid, 2.0 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
As still further aspects of the invention: in the step S31, the raw material C includes: 130 parts of castor oil modified polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 3.5 parts of 2, 2-dihydroxypropionic acid, 2.0 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
Based on the scheme: in the steps S12, S22 and S32, the controlled temperature is 85 ℃, and the reaction time is 5 hours; in the steps S13, S23 and S33, the addition amount of triethylamine is 3 parts, and the stirring treatment time is controlled to be 10 minutes; in the steps S14, S24 and S34, the addition amount of distilled water is 500 parts.
Preferred on the basis of the foregoing scheme: the preparation of the components of the polyurethane heat-conducting pouring sealant comprises the following steps:
s41: uniformly mixing the powder A, the powder B and the powder C, and marking the mixture as mixed powder;
s42: sequentially adding 85g of castor oil modified dihydric alcohol with the number average molecular weight of 2000, 5g of trimethylolpropane, 0.1g of dibutyl tin dilaurate, 0.1g of organosilicon defoamer and 1000g of mixed powder into a container, vacuumizing and uniformly stirring to obtain a polyurethane heat-conducting pouring sealant A component;
s43: 90g of polymeric MDI with 9.8 percent of isocyanate (NCO) weight content, 0.1g of dibutyl tin dilaurate, 0.1g of organosilicon defoamer and 1000g of mixed powder are sequentially added into a container, and the mixture is vacuumized and stirred uniformly to obtain the component B of the polyurethane heat-conducting pouring sealant.
Further preferred on the basis of the foregoing scheme is: in the step S41, powder A, powder B and powder C are mixed according to the weight ratio of 0.75:1: 4.
The beneficial effects of the invention are as follows:
1. according to the invention, polyurethane with a molecular structure similar to or the same as that of polyurethane in the polyurethane heat-conducting pouring sealant is mixed with the heat-conducting powder, and then spray drying is carried out, so that the modified powder with the surface coated with polyurethane macromolecules is obtained, the compatibility of the powder in a polyurethane system is greatly improved, more powder can be filled under the condition of the same viscosity, and the heat-conducting property is improved.
2. The invention uses carboxylic polyurethane emulsion, the salifying agent is triethylamine, the carboxylic acid group exists in the form of carboxylic acid-triethylamine salt under the emulsion state, and after spray drying, polyurethane macromolecules can be wrapped on the surface of powder, so as to achieve the effect of surface treatment. In addition, the salt forming agent triethylamine can volatilize in the spraying process, the hydrophilicity of polyurethane molecules wrapped on the surface of the powder is greatly reduced, and the storage stability of the polyurethane heat conduction pouring sealant is also ensured to a certain extent.
Drawings
FIG. 1 is a graph showing the viscosity contrast of the product in the experiment of the present invention;
FIG. 2 is a graph of thermal conductivity versus product in an experiment of the present invention.
Detailed Description
The technical scheme of the patent is further described in detail below with reference to the specific embodiments.
Example 1:
a surface treatment method of powder for polyurethane heat-conducting pouring sealant comprises the following steps:
s1: preparing carboxylic acid type polyurethane anion emulsion with the molecular structure similar to or the same as that of polyurethane in the polyurethane heat conduction pouring sealant;
s2: uniformly mixing the powder to be treated with the polyurethane emulsion according to a certain proportion;
s3: spraying the mixture by using a spray dryer to obtain powder with the surface modified by polyurethane macromolecules.
The surface treatment method of the powder specifically comprises the following steps:
s11: adding the raw material A into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s12: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s13: adding triethylamine into the polyurethane prepolymer, and stirring;
s14: stirring, and then pouring into distilled water for emulsification and dispersion;
s15: obtaining polyurethane anion emulsion through reduced pressure distillation;
s16: spherical alumina of D502 microns is mixed with the emulsion according to the mass ratio of 1:2, uniformly mixing;
s17: and (3) spray drying to obtain the alumina powder which can be used in the field of polyurethane heat conduction pouring sealant, wherein the alumina powder is named as powder A.
In the step S11, the raw material a includes: 120 parts of liquid polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 4 parts of dimethylol butyric acid, 1.5 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
In the step S12, the temperature is controlled to be 85 ℃, and the reaction time is 5 hours.
In the step S13, the amount of triethylamine added is 3 parts, and the stirring time is controlled to be 10 minutes.
In the step S14, the addition amount of distilled water is 500 parts.
Example 2:
the surface treatment method of the powder for the polyurethane heat-conducting pouring sealant specifically comprises the following steps of:
s21: adding the raw material B into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s22: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s23: adding triethylamine into the polyurethane prepolymer, and stirring;
s24: stirring, and then pouring into distilled water for emulsification and dispersion;
s25: obtaining polyurethane anion emulsion through reduced pressure distillation;
s26: d5010 micrometer aluminum hydroxide and the emulsion are mixed according to the mass ratio of 1:2, uniformly mixing;
s27: and (3) spray drying to obtain aluminum hydroxide which can be used in the field of polyurethane heat conduction pouring sealant, wherein the aluminum hydroxide powder is marked as powder B.
Wherein, in the step S21, the raw material B includes: 130 parts of castor oil modified polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 3.5 parts of 2, 2-dihydroxypropionic acid, 2.0 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
In the step S22, the temperature is controlled to be 85 ℃, and the reaction time is 5 hours.
In the step S23, the amount of triethylamine added is 3 parts, and the stirring time is controlled to be 10 minutes.
In the step S24, the addition amount of distilled water is 500 parts.
Example 3:
the surface treatment method of the powder for the polyurethane heat-conducting pouring sealant specifically comprises the following steps:
s31: adding the raw material C into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s32: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s33: adding triethylamine into the polyurethane prepolymer, and stirring;
s34: stirring, and then pouring into distilled water for emulsification and dispersion;
s35: obtaining polyurethane anion emulsion through reduced pressure distillation;
s36: spherical alumina of D5030 microns is mixed with the emulsion according to the mass ratio of 1:2, uniformly mixing;
s37: and (3) spray drying to obtain the alumina which can be used in the field of polyurethane heat conduction pouring sealant, wherein the alumina powder is named as powder C.
Wherein, in the step S31, the raw material C includes: 130 parts of castor oil modified polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 3.5 parts of 2, 2-dihydroxypropionic acid, 2.0 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
In the step S32, the temperature is controlled to be 85 ℃, and the reaction time is 5 hours.
In the step S33, the amount of triethylamine added is 3 parts, and the stirring time is controlled to be 10 minutes.
In the step S34, the distilled water is added in an amount of 500 parts.
Example 4:
the surface treatment method of the powder for the polyurethane heat-conducting pouring sealant comprises the following steps of:
s41: uniformly mixing the powder A, the powder B and the powder C, and marking the mixture as mixed powder;
s42: sequentially adding 85g of castor oil modified dihydric alcohol with the number average molecular weight of 2000, 5g of trimethylolpropane, 0.1g of dibutyl tin dilaurate, 0.1g of organosilicon defoamer and 1000g of mixed powder into a container, vacuumizing and uniformly stirring to obtain a polyurethane heat-conducting pouring sealant A component;
s43: 90g of polymeric MDI with 9.8 percent of isocyanate (NCO) weight content, 0.1g of dibutyl tin dilaurate, 0.1g of organosilicon defoamer and 1000g of mixed powder are sequentially added into a container, and the mixture is vacuumized and stirred uniformly to obtain the component B of the polyurethane heat-conducting pouring sealant.
In the step S41, the weight ratio of powder a, powder B, and powder C is 0.75:1: 4.
Experiment:
according to the above formulation, comparative experiment 1 was performed using powder not subjected to surface treatment, comparative experiment 2 was performed using powder subjected to surface treatment with KH550, comparative experiment 3 was performed using powder subjected to surface treatment with KH560, and the performance comparative results were as follows:
from the results, the powder obtained by the method can achieve the effects of high filling and low viscosity in a corresponding polyurethane system, and the thermal conductivity coefficient of the prepared polyurethane thermal conductivity pouring sealant can reach about 3.4W/m.K.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The surface treatment method of the powder for the polyurethane heat-conducting pouring sealant is characterized by comprising the following steps of:
s1: preparing carboxylic acid type polyurethane anion emulsion with the molecular structure similar to or the same as that of polyurethane in the polyurethane heat conduction pouring sealant;
s2: uniformly mixing the powder to be treated with the polyurethane emulsion according to a certain proportion;
s3: spraying the mixture by using a spray dryer to obtain powder with the surface modified by polyurethane macromolecules.
2. The surface treatment method of the powder for the polyurethane heat conduction pouring sealant according to claim 1, which is characterized by comprising the following steps:
s11: adding the raw material A into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s12: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s13: adding triethylamine into the polyurethane prepolymer, and stirring;
s14: stirring, and then pouring into distilled water for emulsification and dispersion;
s15: obtaining polyurethane anion emulsion through reduced pressure distillation;
s16: spherical alumina of D502 microns is mixed with the emulsion according to the mass ratio of 1:2, uniformly mixing;
s17: and (3) spray drying to obtain the alumina powder which can be used in the field of polyurethane heat conduction pouring sealant, wherein the alumina powder is named as powder A.
3. The surface treatment method of the powder for the polyurethane heat conduction pouring sealant according to claim 2, which is characterized by comprising the following steps:
s21: adding the raw material B into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s22: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s23: adding triethylamine into the polyurethane prepolymer, and stirring;
s24: stirring, and then pouring into distilled water for emulsification and dispersion;
s25: obtaining polyurethane anion emulsion through reduced pressure distillation;
s26: d5010 micrometer aluminum hydroxide and the emulsion are mixed according to the mass ratio of 1:2, uniformly mixing;
s27: and (3) spray drying to obtain aluminum hydroxide which can be used in the field of polyurethane heat conduction pouring sealant, wherein the aluminum hydroxide powder is marked as powder B.
4. The surface treatment method of the powder for the polyurethane heat conduction pouring sealant according to claim 3, which is characterized by comprising the following steps:
s31: adding the raw material C into a reaction vessel provided with a stirrer and a reflux condenser pipe under the nitrogen environment, and mixing;
s32: after uniform mixing, controlling the temperature, and reacting to obtain polyurethane prepolymer;
s33: adding triethylamine into the polyurethane prepolymer, and stirring;
s34: stirring, and then pouring into distilled water for emulsification and dispersion;
s35: obtaining polyurethane anion emulsion through reduced pressure distillation;
s36: spherical alumina of D5030 microns is mixed with the emulsion according to the mass ratio of 1:2, uniformly mixing;
s37: and (3) spray drying to obtain the alumina which can be used in the field of polyurethane heat conduction pouring sealant, wherein the alumina powder is named as powder C.
5. The method for surface treatment of powder for polyurethane heat-conducting potting adhesive of claim 4, wherein in step S11, the raw material a comprises: 120 parts of liquid polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 4 parts of dimethylol butyric acid, 1.5 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
6. The method for surface treatment of powder for polyurethane heat-conducting potting adhesive of claim 4, wherein in step S21, the raw material B comprises: 130 parts of castor oil modified polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 3.5 parts of 2, 2-dihydroxypropionic acid, 2.0 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
7. The method for surface treatment of powder for polyurethane heat-conducting potting adhesive of claim 4, wherein in step S31, the raw material C comprises: 130 parts of castor oil modified polyether glycol with the number average molecular weight of 2000, 18 parts of toluene diisocyanate, 3.5 parts of 2, 2-dihydroxypropionic acid, 2.0 parts of trimethylolpropane, 27 parts of butanone and 0.1 part of dibutyl tin dilaurate.
8. The surface treatment method of the powder for the polyurethane heat conduction pouring sealant according to any one of claims 4 to 7, wherein in the steps S12, S22 and S32, the controlled temperature is 85 ℃, and the reaction time is 5 hours; in the steps S13, S23 and S33, the addition amount of triethylamine is 3 parts, and the stirring treatment time is controlled to be 10 minutes; in the steps S14, S24 and S34, the addition amount of distilled water is 500 parts.
9. The surface treatment method of the powder for the polyurethane heat-conducting pouring sealant according to claim 8, wherein the preparation of the components of the polyurethane heat-conducting pouring sealant comprises the following steps:
s41: uniformly mixing the powder A, the powder B and the powder C, and marking the mixture as mixed powder;
s42: sequentially adding 85g of castor oil modified dihydric alcohol with the number average molecular weight of 2000, 5g of trimethylolpropane, 0.1g of dibutyl tin dilaurate, 0.1g of organosilicon defoamer and 1000g of mixed powder into a container, vacuumizing and uniformly stirring to obtain a polyurethane heat-conducting pouring sealant A component;
s43: 90g of polymeric MDI with 9.8 percent of isocyanate (NCO) weight content, 0.1g of dibutyl tin dilaurate, 0.1g of organosilicon defoamer and 1000g of mixed powder are sequentially added into a container, and the mixture is vacuumized and stirred uniformly to obtain the component B of the polyurethane heat-conducting pouring sealant.
10. The surface treatment method of the powder for the polyurethane heat conduction pouring sealant according to claim 9, wherein in the step S41, the weight ratio of the powder a to the powder B to the powder C is 0.75:1: 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211559259.0A CN116041983A (en) | 2022-12-06 | 2022-12-06 | Surface treatment method of powder for polyurethane heat-conducting pouring sealant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211559259.0A CN116041983A (en) | 2022-12-06 | 2022-12-06 | Surface treatment method of powder for polyurethane heat-conducting pouring sealant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116041983A true CN116041983A (en) | 2023-05-02 |
Family
ID=86126344
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211559259.0A Pending CN116041983A (en) | 2022-12-06 | 2022-12-06 | Surface treatment method of powder for polyurethane heat-conducting pouring sealant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116041983A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05214054A (en) * | 1992-02-04 | 1993-08-24 | Dainichiseika Color & Chem Mfg Co Ltd | Production of polyurethane and fine exactly spherical polyurethane particle |
| CN102627937A (en) * | 2012-03-27 | 2012-08-08 | 合肥工业大学 | Bi-component conductive polyurethane pouring adhesive and preparation method thereof |
| CN105907348A (en) * | 2016-06-08 | 2016-08-31 | 蚌埠高华电子股份有限公司 | Nanometer aluminum nitride modified composite epoxy pouring sealant for LED display screen |
| CN105969278A (en) * | 2016-06-08 | 2016-09-28 | 蚌埠高华电子股份有限公司 | Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen |
| CN108976353A (en) * | 2018-06-27 | 2018-12-11 | 滁州环球聚氨酯科技有限公司 | A kind of preparation method of multiple modified polyaminoester emulsion |
| CN110028923A (en) * | 2019-04-28 | 2019-07-19 | 安徽匠星联创新材料科技有限公司 | A kind of solvent-free dual-component polyurethane casting glue |
| CN110591158A (en) * | 2019-09-24 | 2019-12-20 | 浙江华峰新材料股份有限公司 | Modified core-shell type aluminum oxide and polyurethane composite material, and preparation method and application thereof |
| CN112812369A (en) * | 2020-12-31 | 2021-05-18 | 金发科技股份有限公司 | Polymer-coated composite hollow microsphere and preparation method and application thereof |
| CN114410268A (en) * | 2021-12-31 | 2022-04-29 | 深圳市安品有机硅材料有限公司 | Magnetic conductive polyurethane pouring sealant and preparation method thereof |
| CN114854354A (en) * | 2022-05-07 | 2022-08-05 | 宁波源成新材料科技有限公司 | Low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and preparation method thereof |
-
2022
- 2022-12-06 CN CN202211559259.0A patent/CN116041983A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05214054A (en) * | 1992-02-04 | 1993-08-24 | Dainichiseika Color & Chem Mfg Co Ltd | Production of polyurethane and fine exactly spherical polyurethane particle |
| CN102627937A (en) * | 2012-03-27 | 2012-08-08 | 合肥工业大学 | Bi-component conductive polyurethane pouring adhesive and preparation method thereof |
| CN105907348A (en) * | 2016-06-08 | 2016-08-31 | 蚌埠高华电子股份有限公司 | Nanometer aluminum nitride modified composite epoxy pouring sealant for LED display screen |
| CN105969278A (en) * | 2016-06-08 | 2016-09-28 | 蚌埠高华电子股份有限公司 | Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen |
| CN108976353A (en) * | 2018-06-27 | 2018-12-11 | 滁州环球聚氨酯科技有限公司 | A kind of preparation method of multiple modified polyaminoester emulsion |
| CN110028923A (en) * | 2019-04-28 | 2019-07-19 | 安徽匠星联创新材料科技有限公司 | A kind of solvent-free dual-component polyurethane casting glue |
| CN110591158A (en) * | 2019-09-24 | 2019-12-20 | 浙江华峰新材料股份有限公司 | Modified core-shell type aluminum oxide and polyurethane composite material, and preparation method and application thereof |
| CN112812369A (en) * | 2020-12-31 | 2021-05-18 | 金发科技股份有限公司 | Polymer-coated composite hollow microsphere and preparation method and application thereof |
| CN114410268A (en) * | 2021-12-31 | 2022-04-29 | 深圳市安品有机硅材料有限公司 | Magnetic conductive polyurethane pouring sealant and preparation method thereof |
| CN114854354A (en) * | 2022-05-07 | 2022-08-05 | 宁波源成新材料科技有限公司 | Low-viscosity flame-retardant heat-conducting solvent-free polyurethane electronic pouring sealant and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高旭瑞;王利魁;姚伯龙;: "光固化水性聚氨酯导热涂层的制备及性能", 材料保护, no. 11, 15 November 2016 (2016-11-15), pages 26 - 31 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11485857B2 (en) | Amino silicone oil-modified elastomer material and preparation method thereof | |
| CN103804689B (en) | A kind of silicone oligomer of the special resistance to anti-soil of polyureas and preparation method thereof | |
| CN115386280B (en) | Heavy-duty anticorrosive paint and preparation method thereof | |
| CN110194930B (en) | High-temperature-resistant and high-cold-resistant coating and application thereof | |
| CN110734739A (en) | Preparation method of organic silicon pressure-sensitive adhesives | |
| CN114479626A (en) | Coating composition | |
| CN112341922A (en) | Zero-solvent high-environmental-protection-performance silane modified polymer waterproof coating and preparation method thereof | |
| CN102786873B (en) | Nano compound anticorrosive paint and preparation method thereof | |
| CN112322162A (en) | Polyurea coating and preparation method thereof | |
| CN116041983A (en) | Surface treatment method of powder for polyurethane heat-conducting pouring sealant | |
| CN111763303A (en) | Water-based blocked polyurethane curing agent and preparation method thereof | |
| CN115074079A (en) | Single-component addition type organic silicon heat-conducting adhesive and preparation method thereof | |
| CN117384584B (en) | Double-component heat-conducting pouring sealant for OBC charging module and preparation method thereof | |
| CN112251165A (en) | Special prime coat-free platinum vulcanizing agent for combination of metal substrate and silica gel and preparation method thereof | |
| CN1047398C (en) | Resin used for cathode electrodeposition paint and its production and application | |
| CN112980376A (en) | Waterborne polyurethane adhesive and preparation method thereof | |
| CN118085717A (en) | A fast-curing material for tower side insulation and preparation method thereof | |
| CN111793365A (en) | Silicon rubber composition and preparation method thereof | |
| KR102364516B1 (en) | Self-healable polyurea/sol-gel silica nanohybrid crosslinked products and method of manufacturing the same | |
| CN1074027C (en) | Preparation of resin emulsion for electrophoretic paint used on thick-film cathode | |
| CN113755083B (en) | Preparation method of solvent-free polyurea coating | |
| CN113861123A (en) | Preparation method of blocked isophorone diisocyanate polymer | |
| CN115433482A (en) | A kind of preparation method of waterborne polyurethane water-resistant coating | |
| CN114958246A (en) | Multifunctional auxiliary agent and preparation method thereof | |
| CN108610935B (en) | Novel single-component moisture-curing polyurethane waterproof coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |