CN105623586A - Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive - Google Patents

Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive Download PDF

Info

Publication number
CN105623586A
CN105623586A CN201511016719.5A CN201511016719A CN105623586A CN 105623586 A CN105623586 A CN 105623586A CN 201511016719 A CN201511016719 A CN 201511016719A CN 105623586 A CN105623586 A CN 105623586A
Authority
CN
China
Prior art keywords
parts
resisting
heat
preparation
expansible black
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
Application number
CN201511016719.5A
Other languages
Chinese (zh)
Inventor
许戈文
熊潜生
霍俊丽
戴震
何纪慧
杨立春
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ANHUI ANDA-HUATAI NEW MATERIAL Co Ltd
Original Assignee
ANHUI ANDA-HUATAI NEW MATERIAL Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by ANHUI ANDA-HUATAI NEW MATERIAL Co Ltd filed Critical ANHUI ANDA-HUATAI NEW MATERIAL Co Ltd
Priority to CN201511016719.5A priority Critical patent/CN105623586A/en
Publication of CN105623586A publication Critical patent/CN105623586A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/06Polyurethanes from polyesters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/10Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C08G18/12Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/4009Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633Compounds of group C08G18/42
    • C08G18/6637Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/664Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633Compounds of group C08G18/42
    • C08G18/6637Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6648Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6651Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666Compounds of group C08G18/48 or C08G18/52
    • C08G18/667Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6674Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666Compounds of group C08G18/48 or C08G18/52
    • C08G18/667Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6685Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/73Polyisocyanates or polyisothiocyanates acyclic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention discloses a preparation method of a heat-resisting and weather-resisting polyurethane embedding adhesive. The preparation method comprises the following steps of reacting acidified expandable graphite with hexamethylene diisocyanate and nano titanium dioxide to obtain modified expandable graphite; mixing hydroxyl-terminated polyethylene glycol adipate, polyhexamethylene adipate glycol and hydroxypropyl polydimethylsiloxane, and then reacting a mixture with the hexamethylene diisocyanate and the modified expandable graphite; adding dioctyl phthalate, dioctyl adipate, dibutyl tin dialurate, tetrabutyl titanate, liquid styrene butadiene rubber, liquid acrylonitrile butadiene rubber, 2-(2minute-hydroxy-3minute,5 minute - dipentylphenyl)benzotriazole and bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate and reacting to obtain a polyurethane prepolymer; adding the polyurethane prepolymer into a chain extender for reacting. The preparation method of the heat-resisting and weather-resisting polyurethane embedding adhesive, provided by the invention, is simple in process and mild in conditions; the obtained embedding adhesive is good in bonding strength, heat resistance and weather resistance.

Description

The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant
Technical field
The present invention relates to polyurethanes technology field, particularly relate to the preparation method of a kind of heat-resisting weatherable polyurethane joint sealant.
Background technology
Joint sealant is mainly used in the bonding of field of electronic components in electronic equipment; also known as electronic pastes; it belongs to liquid before not solidifying; there is mobility; waterproof and dampproof, dust-proof, insulation, heat conduction, secrecy, protection against corrosion, heatproof, shockproof effect can be played after solidification, can be used for bonding, the sealing of electronic devices and components, embedding and coating protection. What use was maximum at present mainly contains epoxy resin embedding adhesive, silicone resin joint sealant and polyurethane pouring sealant.
Urethane can have higher elasticity and intensity in wider durometer level; it has excellent wear resistance, oil-proofness, resistance to fatigue, anti-vibration resistance, water tolerance, electrical insulating property, cheap price in addition; it is made to be widely used in sealing and the protection field of the components and parts in various field; but polyurethane heat resistant ageing resistance is not good enough, in the process used, there is thermotolerance and the shortcoming of weathering resistance deficiency.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes the preparation method of a kind of heat-resisting weatherable polyurethane joint sealant, its process is simple, mild condition, and cost is low, the joint sealant cohesive strength height obtained, and thermotolerance and good weatherability.
The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant that the present invention proposes, comprises the following steps:
S1, by weight by 50-100 part massfraction be 98.3% sulfuric acid and 20-40 part massfraction be 65% nitric acid mix and obtain mixing acid, 3-5 part expansible black lead is added after being cooled to room temperature, ultrasonic 20-50min, 0.5-1.5h is stirred after being warming up to 90-100 DEG C, then the dilution of 2000-3000 part water is added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 2-5 part HDI is mixed with 35-50 part anhydrous propanone and obtain material A, 4-6 part acidifying expansible black lead is added in 10-25 part anhydrous propanone and mixes, then material A and 3-10 part nano titanium oxide is added, stirring reaction 20-45min at 30-45 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 20-35 part terminal hydroxy group polyethylene glycol adipate glycol, 30-60 part polyhexamethylene adipate glycol and 5-15 part hydroxypropyl polydimethylsiloxane mix, then 15-25 part HDI and 3-15 part modification expansible black lead is added, 1-1.5h is reacted at 70-85 DEG C, add 2-5 part dioctyl phthalate (DOP) again, 1-5 part adipic acid dioctyl ester, 0.1-0.5 part dibutyl tin laurate, 0.1-0.5 part tetrabutyl titanate, 3-10 part liquid styrene butadiene rubber, 2-10 part liquid acrylonitrile butadiene rubber, 0.1-0.8 part 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.1-0.8 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1-2.5h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 3-5min under the rotating speed of 100-200r/min, then adding 5-12 part chainextender, under the stirring velocity of 100-200r/min, stirring reaction 15-25min obtains described heat-resisting weatherable polyurethane joint sealant.
Preferably, in S1, the weight ratio of HDI, acidifying expansible black lead and nano titanium oxide is 3-4.5:5-6:5-9.
Preferably, in S2, terminal hydroxy group polyethylene glycol adipate glycol, polyhexamethylene adipate glycol, hydroxypropyl polydimethylsiloxane, HDI, modification expansible black lead, dioctyl phthalate (DOP), adipic acid dioctyl ester, dibutyl tin laurate, tetrabutyl titanate, liquid styrene butadiene rubber, liquid acrylonitrile butadiene rubber, 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and two (2, 2, 6, 6-tetramethyl--4-piperidyl) weight ratio of sebate is 25-32:40-55:7-12:19-22:7-11:3-4:3.2-4:0.32-0.4:0.32-0.4: 5.6-7:5-6:0.3-0.4:0.25-0.5.
Preferably, in S2, under the protection of nitrogen, by weight by 30 parts of terminal hydroxy group polyethylene glycol adipate glycol, 46 parts of polyhexamethylene adipate glycols and 10 parts of hydroxypropyl polydimethylsiloxanes mix, then 20 parts of HDI and 10 parts of modification expansible black leads are added, 1.5h is reacted at 80 DEG C, add 3.6 parts of dioctyl phthalate (DOP)s again, 3.5 parts of adipic acid dioctyl esters, 0.38 part of dibutyl tin laurate, 0.35 part of tetrabutyl titanate, 6.5 parts of liquid styrene butadiene rubbers, 5.6 parts of liquid acrylonitrile butadiene rubber, 0.35 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.42 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1.8h, obtain base polyurethane prepolymer for use as.
Preferably, in S3, the weight ratio of base polyurethane prepolymer for use as, chainextender is 100:8-11.
Preferably, in S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 4min under the rotating speed of 150r/min, then adding 10 parts of chainextenders, under the stirring velocity of 180r/min, stirring reaction 22min obtains described heat-resisting weatherable polyurethane joint sealant.
Preferably, in S3, described chainextender is 1,6-hexylene glycol, glycerine, TriMethylolPropane(TMP), glycol ether, triglycol, neopentyl glycol, diethylaminoethanol, diethyl toluene diamine, triethylenediamine, 4,4 '-diamino-3, one or more mixture in 3 '-dichloro diphenyl methane, tetramethylolmethane, Resorcinol two (beta-hydroxyethyl) ether, N, N-dimethyl benzylamine.
In the present invention, first have selected the mixing acid of nitric acid and sulfuric acid expansible black lead has been carried out acidification reaction to obtain acidifying expansible black lead, thus a large amount of hydroxyls and carboxyl isoreactivity group is introduced on the surface of expansible black lead, add HDI afterwards and acidifying expansible black lead has been carried out modification, thus isocyanic ester has been incorporated into the surface of expansible black lead, after adding nano titanium oxide, nano titanium oxide creates effect by the active group of the hydroxyl on surface and expansible black lead surface, thus the surface that nano titanium oxide has been dispersed in expansible black lead obtains modification expansible black lead, afterwards in the preparation process of base polyurethane prepolymer for use as, add HDI and modification expansible black lead, its modification expansible black lead surface is containing the group identical with HDI, therefore modification expansible black lead is uniformly dispersed in system, the flame retardant resistance significantly improving joint sealant and thermotolerance is coordinated with hydroxypropyl polydimethylsiloxane, with 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate cooperation, significantly improve weathering resistance and the ultraviolet light stability of joint sealant, give joint sealant certain germ resistance simultaneously, in addition, system adds liquid styrene butadiene rubber and liquid acrylonitrile butadiene rubber, improve the mechanical strength of urethane, improve the stripping strength of joint sealant simultaneously, and reduce cost.
Embodiment
Below, by specific embodiment, the technical scheme of the present invention is described in detail.
Embodiment 1
The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant that the present invention proposes, comprises the following steps:
S1, by weight by 100 parts of massfractions be 98.3% sulfuric acid and 20 parts of massfractions be 65% nitric acid mix and obtain mixing acid, 5 parts of expansible black leads are added after being cooled to room temperature, ultrasonic 20min, 0.5h is stirred after being warming up to 100 DEG C, then 3000 parts of water dilutions are added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 5 parts of HDI are mixed with 50 parts of anhydrous propanones and obtain material A, 4 parts of acidifying expansible black leads are added in 25 parts of anhydrous propanones and mixes, then material A and 3 parts of nano titanium oxides are added, stirring reaction 20min at 45 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 20 parts of terminal hydroxy group polyethylene glycol adipate glycol, 60 parts of polyhexamethylene adipate glycols and 5 parts of hydroxypropyl polydimethylsiloxanes mix, then 25 parts of HDI and 3 parts of modification expansible black leads are added, 1h is reacted at 85 DEG C, add 5 parts of dioctyl phthalate (DOP)s again, 1 part of adipic acid dioctyl ester, 0.5 part of dibutyl tin laurate, 0.1 part of tetrabutyl titanate, 10 parts of liquid styrene butadiene rubbers, 2 parts of liquid acrylonitrile butadiene rubber, 0.8 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.1 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 2.5h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 5min under the rotating speed of 100r/min, then adding 5 parts of chainextenders, under the stirring velocity of 200r/min, stirring reaction 15min obtains described heat-resisting weatherable polyurethane joint sealant.
Embodiment 2
The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant that the present invention proposes, comprises the following steps:
S1, by weight by 50 parts of massfractions be 98.3% sulfuric acid and 40 parts of massfractions be 65% nitric acid mix and obtain mixing acid, 3 parts of expansible black leads are added after being cooled to room temperature, ultrasonic 50min, 1.5h is stirred after being warming up to 90 DEG C, then 2000 parts of water dilutions are added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 5 parts of HDI are mixed with 35 parts of anhydrous propanones and obtain material A, 6 parts of acidifying expansible black leads are added in 10 parts of anhydrous propanones and mixes, then material A and 10 parts of nano titanium oxides are added, stirring reaction 45min at 30 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 35 parts of terminal hydroxy group polyethylene glycol adipate glycol, 30 parts of polyhexamethylene adipate glycols and 15 parts of hydroxypropyl polydimethylsiloxanes mix, then 15 parts of HDI and 15 parts of modification expansible black leads are added, 1.5h is reacted at 70 DEG C, add 2 parts of dioctyl phthalate (DOP)s again, 5 parts of adipic acid dioctyl esters, 0.1 part of dibutyl tin laurate, 0.5 part of tetrabutyl titanate, 3 parts of liquid styrene butadiene rubbers, 10 parts of liquid acrylonitrile butadiene rubber, 0.1 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.8 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 3min under the rotating speed of 200r/min, then adding 12 parts of triethylenediamines, under the stirring velocity of 100r/min, stirring reaction 25min obtains described heat-resisting weatherable polyurethane joint sealant.
Embodiment 3
The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant that the present invention proposes, comprises the following steps:
S1, by weight by 65 parts of massfractions be 98.3% sulfuric acid and 36 parts of massfractions be 65% nitric acid mix and obtain mixing acid, 3.6 parts of expansible black leads are added after being cooled to room temperature, ultrasonic 45min, 1.2h is stirred after being warming up to 93 DEG C, then 2350 parts of water dilutions are added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 4.5 parts of HDI are mixed with 40 parts of anhydrous propanones and obtain material A, 6 parts of acidifying expansible black leads are added in 13 parts of anhydrous propanones and mixes, then material A and 9 parts of nano titanium oxides are added, stirring reaction 40min at 38 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 25 parts of terminal hydroxy group polyethylene glycol adipate glycol, 55 parts of polyhexamethylene adipate glycols and 7 parts of hydroxypropyl polydimethylsiloxanes mix, then 22 parts of HDI and 7 parts of modification expansible black leads are added, 1.1h is reacted at 82 DEG C, add 4 parts of dioctyl phthalate (DOP)s again, 3.2 parts of adipic acid dioctyl esters, 0.4 part of dibutyl tin laurate, 0.32 part of tetrabutyl titanate, 7 parts of liquid styrene butadiene rubbers, 5 parts of liquid acrylonitrile butadiene rubber, 0.4 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.25 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 2.1h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 4.2min under the rotating speed of 130r/min, then 4 parts of Resorcinol two (beta-hydroxyethyl) ether, 4 parts of N are added, N-dimethyl benzylamine, under the stirring velocity of 170r/min, stirring reaction 18min obtains described heat-resisting weatherable polyurethane joint sealant.
Embodiment 4
The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant that the present invention proposes, comprises the following steps:
S1, by weight by 80 parts of massfractions be 98.3% sulfuric acid and 28 parts of massfractions be 65% nitric acid mix and obtain mixing acid, 4.3 parts of expansible black leads are added after being cooled to room temperature, ultrasonic 30min, 0.8h is stirred after being warming up to 97 DEG C, then 2800 parts of water dilutions are added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 3 parts of HDI are mixed with 47 parts of anhydrous propanones and obtain material A, 5 parts of acidifying expansible black leads are added in 22 parts of anhydrous propanones and mixes, then material A and 5 parts of nano titanium oxides are added, stirring reaction 26min at 42 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 32 parts of terminal hydroxy group polyethylene glycol adipate glycol, 40 parts of polyhexamethylene adipate glycols and 12 parts of hydroxypropyl polydimethylsiloxanes mix, then 19 parts of HDI and 11 parts of modification expansible black leads are added, 1.3h is reacted at 76 DEG C, add 3 parts of dioctyl phthalate (DOP)s again, 4 parts of adipic acid dioctyl esters, 0.32 part of dibutyl tin laurate, 0.4 part of tetrabutyl titanate, 5.6 parts of liquid styrene butadiene rubbers, 6 parts of liquid acrylonitrile butadiene rubber, 0.3 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.5 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1.3h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 3.5min under the rotating speed of 180r/min, then adding 4 parts of triglycols, 2 parts of neopentyl glycol, 5 portions of diethylaminoethanols, under the stirring velocity of 135r/min, stirring reaction 21min obtains described heat-resisting weatherable polyurethane joint sealant.
Embodiment 5
The preparation method of a kind of heat-resisting weatherable polyurethane joint sealant that the present invention proposes, comprises the following steps:
S1, by weight by 85 parts of massfractions be 98.3% sulfuric acid and 36 parts of massfractions be 65% nitric acid mix and obtain mixing acid, 4 parts of expansible black leads are added after being cooled to room temperature, ultrasonic 35min, 1h is stirred after being warming up to 98 DEG C, then 2500 parts of water dilutions are added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 5.5 parts of HDI are mixed with 42 parts of anhydrous propanones and obtain material A, 5.3 parts of acidifying expansible black leads are added in 20 parts of anhydrous propanones and mixes, then material A and 7 parts of nano titanium oxides are added, stirring reaction 30min at 40 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 30 parts of terminal hydroxy group polyethylene glycol adipate glycol, 46 parts of polyhexamethylene adipate glycols and 10 parts of hydroxypropyl polydimethylsiloxanes mix, then 20 parts of HDI and 10 parts of modification expansible black leads are added, 1.5h is reacted at 80 DEG C, add 3.6 parts of dioctyl phthalate (DOP)s again, 3.5 parts of adipic acid dioctyl esters, 0.38 part of dibutyl tin laurate, 0.35 part of tetrabutyl titanate, 6.5 parts of liquid styrene butadiene rubbers, 5.6 parts of liquid acrylonitrile butadiene rubber, 0.35 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.42 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1.8h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 4min under the rotating speed of 150r/min, then adding 10 parts of 1,6-HDs, under the stirring velocity of 180r/min, stirring reaction 22min obtains described heat-resisting weatherable polyurethane joint sealant.
The above; it is only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; any it is familiar with those skilled in the art in the technical scope that the present invention discloses; technical scheme and invention design thereof according to the present invention are equal to replacement or are changed, and all should be encompassed within protection scope of the present invention.

Claims (7)

1. the preparation method of a heat-resisting weatherable polyurethane joint sealant, it is characterised in that, comprise the following steps:
S1, by weight by 50-100 part massfraction be 98.3% sulfuric acid and 20-40 part massfraction be 65% nitric acid mix and obtain mixing acid, 3-5 part expansible black lead is added after being cooled to room temperature, ultrasonic 20-50min, 0.5-1.5h is stirred after being warming up to 90-100 DEG C, then the dilution of 2000-3000 part water is added, standing final vacuum takes out filter, and washing obtains acidifying expansible black lead to neutral post-drying; By weight 2-5 part HDI is mixed with 35-50 part anhydrous propanone and obtain material A, 4-6 part acidifying expansible black lead is added in 10-25 part anhydrous propanone and mixes, then material A and 3-10 part nano titanium oxide is added, stirring reaction 20-45min at 30-45 DEG C, reaction obtains modification expansible black lead through filtration, drying after terminating;
S2, under the protection of nitrogen, by weight by 20-35 part terminal hydroxy group polyethylene glycol adipate glycol, 30-60 part polyhexamethylene adipate glycol and 5-15 part hydroxypropyl polydimethylsiloxane mix, then 15-25 part HDI and 3-15 part modification expansible black lead is added, 1-1.5h is reacted at 70-85 DEG C, add 2-5 part dioctyl phthalate (DOP) again, 1-5 part adipic acid dioctyl ester, 0.1-0.5 part dibutyl tin laurate, 0.1-0.5 part tetrabutyl titanate, 3-10 part liquid styrene butadiene rubber, 2-10 part liquid acrylonitrile butadiene rubber, 0.1-0.8 part 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.1-0.8 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1-2.5h, obtain base polyurethane prepolymer for use as,
S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 3-5min under the rotating speed of 100-200r/min, then adding 5-12 part chainextender, under the stirring velocity of 100-200r/min, stirring reaction 15-25min obtains described heat-resisting weatherable polyurethane joint sealant.
2. the preparation method of heat-resisting weatherable polyurethane joint sealant according to claim 1, it is characterised in that, in S1, the weight ratio of HDI, acidifying expansible black lead and nano titanium oxide is 3-4.5:5-6:5-9.
3. the preparation method of heat-resisting weatherable polyurethane joint sealant according to claim 1 or 2, it is characterized in that, in S2, terminal hydroxy group polyethylene glycol adipate glycol, polyhexamethylene adipate glycol, hydroxypropyl polydimethylsiloxane, HDI, modification expansible black lead, dioctyl phthalate (DOP), adipic acid dioctyl ester, dibutyl tin laurate, tetrabutyl titanate, liquid styrene butadiene rubber, liquid acrylonitrile butadiene rubber, 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and two (2, 2, 6, 6-tetramethyl--4-piperidyl) weight ratio of sebate is 25-32:40-55:7-12:19-22:7-11:3-4:3.2-4:0.32-0.4:0.32-0.4: 5.6-7:5-6:0.3-0.4:0.25-0.5.
4. the preparation method of heat-resisting weatherable polyurethane joint sealant according to any one of claim 1-3, it is characterized in that, in S2, under the protection of nitrogen, by weight by 30 parts of terminal hydroxy group polyethylene glycol adipate glycol, 46 parts of polyhexamethylene adipate glycols and 10 parts of hydroxypropyl polydimethylsiloxanes mix, then 20 parts of HDI and 10 parts of modification expansible black leads are added, 1.5h is reacted at 80 DEG C, add 3.6 parts of dioctyl phthalate (DOP)s again, 3.5 parts of adipic acid dioctyl esters, 0.38 part of dibutyl tin laurate, 0.35 part of tetrabutyl titanate, 6.5 parts of liquid styrene butadiene rubbers, 5.6 parts of liquid acrylonitrile butadiene rubber, 0.35 part of 2-(2 '-hydroxyl-3 ', 5 '-diamyl phenyl) benzotriazole and 0.42 part two (2, 2, 6, 6-tetramethyl--4-piperidyl) sebate stirring reaction 1.8h, obtain base polyurethane prepolymer for use as.
5. the preparation method of heat-resisting weatherable polyurethane joint sealant according to any one of claim 1-4, it is characterised in that, in S3, the weight ratio of base polyurethane prepolymer for use as, chainextender is 100:8-11.
6. the preparation method of heat-resisting weatherable polyurethane joint sealant according to any one of claim 1-5, it is characterized in that, in S3, by weight by 100 parts of base polyurethane prepolymer for use as centrifugal 4min under the rotating speed of 150r/min, then adding 10 parts of chainextenders, under the stirring velocity of 180r/min, stirring reaction 22min obtains described heat-resisting weatherable polyurethane joint sealant.
7. the preparation method of heat-resisting weatherable polyurethane joint sealant according to any one of claim 1-6, it is characterized in that, in S3, described chainextender is 1,6-hexylene glycol, glycerine, TriMethylolPropane(TMP), glycol ether, triglycol, neopentyl glycol, diethylaminoethanol, diethyl toluene diamine, triethylenediamine, 4,4 '-diamino-3, one or more mixture in 3 '-dichloro diphenyl methane, tetramethylolmethane, Resorcinol two (beta-hydroxyethyl) ether, N, N-dimethyl benzylamine.
CN201511016719.5A 2015-12-29 2015-12-29 Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive Pending CN105623586A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201511016719.5A CN105623586A (en) 2015-12-29 2015-12-29 Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201511016719.5A CN105623586A (en) 2015-12-29 2015-12-29 Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive

Publications (1)

Publication Number Publication Date
CN105623586A true CN105623586A (en) 2016-06-01

Family

ID=56038950

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201511016719.5A Pending CN105623586A (en) 2015-12-29 2015-12-29 Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive

Country Status (1)

Country Link
CN (1) CN105623586A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106084750A (en) * 2016-06-21 2016-11-09 秦廷廷 A kind of anti-reflection organic silicon modified polyurethane glue being applied to LED plant growth lamp chip package
CN106085335A (en) * 2016-06-21 2016-11-09 秦廷廷 A kind of organic silicon modified polyurethane heat conduction condensing film being applied to LED plant growth lamp chip package
CN106893142A (en) * 2017-03-10 2017-06-27 北京理工大学 Surface coating has expansible graphite and its manufacture method, the polymer of titania aerogel
CN108587546A (en) * 2018-04-20 2018-09-28 湖州丘天电子科技有限公司 A kind of integrated circuit board embedding adhesive and preparation method thereof
CN108666463A (en) * 2017-03-29 2018-10-16 孚能科技(赣州)有限公司 Casting glue and battery pack
CN112297554A (en) * 2019-08-02 2021-02-02 李海燕 Hot-pressing color-changing laminated structure
CN113861381A (en) * 2021-10-13 2021-12-31 东莞市宏达聚氨酯有限公司 Polyurethane pouring sealant and preparation method thereof
CN114714691A (en) * 2022-05-06 2022-07-08 安徽鼎奂节能科技有限公司 Novel ceramic integrated plate and processing technology thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
夏兆路等: "尼龙6/功能化热膨胀石墨复合材料的制备和性能", 《工程塑料应用》 *
徐阳等: "表面改性对可膨胀石墨填充PP/TPU复合材料的结晶行为、燃烧与力学性能的影响", 《功能材料》 *
李丽娟: "聚氨酯阻燃材料及其应用", 《化工新型材料》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106084750A (en) * 2016-06-21 2016-11-09 秦廷廷 A kind of anti-reflection organic silicon modified polyurethane glue being applied to LED plant growth lamp chip package
CN106085335A (en) * 2016-06-21 2016-11-09 秦廷廷 A kind of organic silicon modified polyurethane heat conduction condensing film being applied to LED plant growth lamp chip package
CN106893142A (en) * 2017-03-10 2017-06-27 北京理工大学 Surface coating has expansible graphite and its manufacture method, the polymer of titania aerogel
CN108666463A (en) * 2017-03-29 2018-10-16 孚能科技(赣州)有限公司 Casting glue and battery pack
CN108587546A (en) * 2018-04-20 2018-09-28 湖州丘天电子科技有限公司 A kind of integrated circuit board embedding adhesive and preparation method thereof
CN112297554A (en) * 2019-08-02 2021-02-02 李海燕 Hot-pressing color-changing laminated structure
CN113861381A (en) * 2021-10-13 2021-12-31 东莞市宏达聚氨酯有限公司 Polyurethane pouring sealant and preparation method thereof
CN114714691A (en) * 2022-05-06 2022-07-08 安徽鼎奂节能科技有限公司 Novel ceramic integrated plate and processing technology thereof

Similar Documents

Publication Publication Date Title
CN105623586A (en) Preparation method of heat-resisting and weather-resisting polyurethane embedding adhesive
CN107892900B (en) Low-modulus high-resilience single-component silane modified polyether sealant and preparation method thereof
CN101818039B (en) Single-component low-modulus polyurethane building sealant and preparation method thereof
US9080087B2 (en) Reduction in modulus of polyurethane sealants and adhesives
CN104292412A (en) Cellulose base polyurethane prepolymer as well as sealing material using cellulose base polyurethane prepolymer, preparation method and application of cellulose base polyurethane prepolymer
KR101097784B1 (en) Structure for complex heat insulator waterproof and method using the same
CN105175674A (en) High hardness and high toughness polyurethane casting adhesive and application thereof
CN110157307B (en) Low-temperature fast-curing polyurea coating and preparation method thereof
CN103224741A (en) Novel nano TiO2/PTFE hybrid fluorocarbon paint applied for resisting pollution flashover of insulators, and preparation method thereof
CN101987950A (en) Single-component polyurethane termite-resistant building sealant
CN101838458B (en) Method for manufacturing polyurethane microporous automotive buffer block
JP2017043740A (en) High strength two-pack environmental response urethane waterproof material composition for hand coating, and urethane waterproof process
CN112852299A (en) Reactive non-cured rubber asphalt waterproof coating and preparation method thereof
CN101781518A (en) Single component colour polyurethane waterproof paint and preparation method thereof
CN112708340A (en) Anti-sagging single-component polyurethane waterproof coating capable of being sprayed and constructed
CN105505282A (en) Quick dry type polyurethane sealant and preparation method thereof
CN108117760A (en) A kind of charging system for electric automobile Acidproof cable material and preparation method thereof
CN106085190A (en) A kind of modified aqueous polyurethane heat-conductive coating for power distribution cabinet and preparation method thereof
CN110003795B (en) Heating-free asphalt-based non-cured waterproof coating and preparation and construction method thereof
CN105038273A (en) Silica gel asphalt waterproof coiled material
JP2018172518A (en) Two-liquid type urethane waterproof material composition for hand coating
CN104861666A (en) Improved antioxidant asphalt waterproof coiled material
KR20130096928A (en) Structure for complex heat insulator waterproof using rubber asphalt sheet coated with non-solvent type urethane and method using the same
CN105038275A (en) Lightweight bituminous waterproof sheet material
CN105038269A (en) Fiber-reinforced bituminous waterproof sheet material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160601

RJ01 Rejection of invention patent application after publication