CN104513352B - A kind of preparation method of single-component cranny filler of polyurethane foam - Google Patents

A kind of preparation method of single-component cranny filler of polyurethane foam Download PDF

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Publication number
CN104513352B
CN104513352B CN201410773472.0A CN201410773472A CN104513352B CN 104513352 B CN104513352 B CN 104513352B CN 201410773472 A CN201410773472 A CN 201410773472A CN 104513352 B CN104513352 B CN 104513352B
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preparation
foam
polyurethane foam
cranny filler
composite catalyst
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CN104513352A (en
Inventor
张洪秀
杨录新
高俊
苏畅
张磊
周颖
刘连茹
陈海云
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Tianyuan (Yichang) new Mstar Technology Ltd
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YINGKOU TANYUN CHEMICALS RESEARCH INSTITUTE CORP
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/161—Catalysts containing two or more components to be covered by at least two of the groups C08G18/166, C08G18/18 or C08G18/22
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/166—Catalysts not provided for in the groups C08G18/18 - C08G18/26
    • C08G18/168—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/18—Catalysts containing secondary or tertiary amines or salts thereof
    • C08G18/20—Heterocyclic amines; Salts thereof
    • C08G18/2045—Heterocyclic amines; Salts thereof containing condensed heterocyclic rings
    • C08G18/2063—Heterocyclic amines; Salts thereof containing condensed heterocyclic rings having two nitrogen atoms in the condensed ring system
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/18—Catalysts containing secondary or tertiary amines or salts thereof
    • C08G18/20—Heterocyclic amines; Salts thereof
    • C08G18/2081—Heterocyclic amines; Salts thereof containing at least two non-condensed heterocyclic rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/141—Hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2101/00—Manufacture of cellular products
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • 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
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/08—Polyurethanes from polyethers

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

A kind of preparation method of single-component cranny filler of polyurethane foam, is related to the preparation method of single-component cranny filler of polyurethane foam, specifically a kind of preparation method that can realize one step foaming and the single-component cranny filler of polyurethane foam with overlength linear meter.Including the synthesis of composite catalyst, the preparation of combined polyether and product.The inventive method is simple, it is easy to implement.The present invention uses dual catalytic agent, strengthens gel catalytic action, can promote to spray the sizing of foam rapid curing.Realize that one step foaming is shaped.Using the method and hydroxyl, the polyalcohol and polymer reaction of amino that add coupling agent, the solidification that the silane group with moisturecuring mechanism of crosslinking accelerates foam is obtained.Using organic solvent is added, material viscosity is reduced, reduce Unit Foam material density, under composite catalyst and the effect of coupling agent fast reaction curing molding, improve foam linear meter number.So that constructing operation and spray volume are easy to control, cost of labor is saved；Meanwhile, the foam volume for spraying foam is increased, increase construction area is 1.39~1.89 times of common gap filler, reduces material cost, solves the problems, such as existing product.

Description

A kind of preparation method of single-component cranny filler of polyurethane foam
Technical field
The present invention relates to the preparation method of single-component cranny filler of polyurethane foam, specifically one kind can realize one step foaming With the preparation method of the single-component cranny filler of polyurethane foam with overlength linear meter.
Technical background
Single-component cranny filler of polyurethane foam is with list by components such as base polyurethane prepolymer for use as, catalyst, foaming agent, propellants A kind of special polyurethane products of branch inhalator jar form package storage.Existing foamed glue product can instantaneously spray bubble when in use The polyurethane materials of foam shape, under pressure foam material can expand, that is, one step foaming is realized, then in absorption air In moisture after, carry out after reaction releases carbon dioxide, then carrying out second time of foaming, foam reaches filling sealing and builds by solidification Build seam or hole or suit doors install the purpose for bonding, fixing.
Due in preparation method, foaming process need to enter the single-component cranny filler of polyurethane foam for being used at present Row 2 times, first time foam overrun is only below 30%, and moisture that need be in absorption air could expansion curing, shape completely Into second time of foaming expansion, continuation expansion rate is more than 70%.Therefore, workmen is advisable the palm that be not easy very much to spraying how many material Hold and control, such as spray material excess, unnecessary expander will be produced, influence construction effect, need cut away, cause material The increasing of cost and cost of labor.
The content of the invention
For above-mentioned situation, it is an object of the invention to provide a kind of single-component cranny filler of polyurethane foam of one step foaming Preparation method.The method is using composite catalyst and adds coupling agent, it is possible to increase frothy gel speed, rapid shaping, and adds Entering organic solvent makes single-component cranny filler of polyurethane foam in construction usage, sprays foam and expands fixation rapidly, can be once Foaming and setting 90-100%, and expansion rate is high, increases foam volume.
The present invention includes for the used technical scheme that solves the above problems；The preparation of composite catalyst, combined polyether Preparation and the preparation of cranny filler of polyurethane foam.
1st, the preparation of composite catalyst
Formula：
Composition specification weight ratio
2 methyl caproic acid technical grade 60-80g
1,8- diazabicylo-bicyclic (5,4,0) -7- hendecene technical grades 70-80g
Preparation method
2 methyl caproic acid is proportionally added into there-necked flask, stirring is opened.1,8- phenodiazines are being added dropwise at 10-15 DEG C of temperature Miscellaneous two ring-bicyclic (5,4,0) -7- hendecenes, time for adding 25~35 minutes.It is warming up to 85~95 DEG C, the reaction time 1.5~ 2.5 hours, room temperature is down to, filtered, obtain composite catalyst.
2nd, the preparation of combined polyether
Formula：
2,2- dual-morpholinyl diethyl ethers above are catalyst；3- isocyanates propyl trimethoxy silicane is coupling Agent；Dichloromethane is organic solvent；Chlorinated paraffin -52 is auxiliary agent.
Preparation method
In there-necked flask, after formula sequentially adds various raw materials more than, it is stirred at room temperature 1 hour, is made combination Polyethers.
3rd, the preparation of cranny filler of polyurethane foam
Technical formula
Preparation method
Combined polyether, polymethylene multi-phenenyl isocyanate, dimethyl ether, the third butane that will be made are being filled by formula rate It is filling into single-component cranny filler of polyurethane foam finished product in installation.
The inventive method is simple, it is easy to implement.The method for using composite catalyst.Traditional monocomponent polyurethane bubble The catalyst that foam gap filler is used is only 2,2- dual-morpholinyl diethyl ethers.The present invention adds self-control composite catalyst and 2,2- double Morpholinyl Anaesthetie Ether is dual catalyst, strengthens gel catalytic action, can promote to spray the sizing of foam rapid curing.
Method using coupling agent is added.Addition 3- isocyanates propyl trimethoxy silicane and hydroxyl, amino it is many First alcohol and polymer reaction, obtain the solidification that the silane group with moisturecuring mechanism of crosslinking accelerates foam.
Using organic solvent is added, material viscosity is reduced, Unit Foam material density is reduced, in composite catalyst and coupling Under the effect of agent fast reaction curing molding, foam linear meter number is improved.By 750ml specifications sealing agent of single component polyurethane foam ratio Compared with；4cm is wide for shaping, and foam hair body 3cm high, product of the present invention can spray 32-34 meters long.And existing common monocomponent polyurethane Foam gap filler is only 18-23 meters.Second time of foaming expansion band is carried out due to avoiding the moisture sprayed in foam re-absorption air The waste for coming, shaping speed is fast, allows for constructing operation and spray volume is easy to control, saves cost of labor；Meanwhile, increased spray Go out the foam volume of foam, increase construction area is 1.39~1.89 times of common gap filler, material cost is reduced, so as to drop Low construction cost.Solve the problems, such as existing product.
The present invention is without accompanying drawing
Specific embodiment
The present invention is described in further detail with reference to embodiment
Embodiment 1
Synthesis composite catalyst
Equipped with constant temperature water bath apparatus, and equipped with thermometer, dropping funel, churned mechanically 200ml there-necked flasks in, plus Enter 65.6 grams of 2 methyl caproic acids, open stirring.In dropping funel, 1,8- diazabicylos-bicyclic (5,4,0) -7- ten is added One 77 grams of alkene, in 10 DEG C of temperature of control, is slowly added dropwise in there-necked flask, and drop finishes within 30 minutes.90 DEG C are warming up to, after reacting 2 hours, Room temperature is cooled to, is filtered, obtain composite catalyst.
The preparation of combined polyether
Formula：
Preparation method
In the there-necked flask of 500ml, after formula sequentially adds various raw materials more than, at room temperature, stir 1 hour.
It is made combined polyether.
The preparation of cranny filler of polyurethane foam
In 750mL inhalator jars, combined polyether 300g, polymethylene multi-phenenyl isocyanate 240g are added, then in gas Filling dimethyl ether 60g on mist agent bottle placer, the third butane 75g, shake 3min, 24h is placed at room temperature and is got product.
The single-component cranny filler of polyurethane foam made draws a design one step foaming amount for 96%；Get foam 4cm wide, 3cm Height, linear meter is 33 meters long, is shown in Table 1.
Embodiment 2
Synthesis composite catalyst
Equipped with constant temperature water bath apparatus, and equipped with thermometer, dropping funel, churned mechanically 200ml there-necked flasks in, plus Enter 65.6 grams of 2 methyl caproic acids, open stirring.In dropping funel, 1,8- diazabicylos-bicyclic (5,4,0) -7- ten is added One 77 grams of alkene, in the case where 14 DEG C of temperature is controlled, is slowly added dropwise in there-necked flask, and drop finishes within 28 minutes.85 DEG C are warming up to, are reacted 2 hours Afterwards, room temperature is cooled to, is filtered, obtain composite catalyst.
The preparation of combined polyether
Formula：
Preparation method
In the there-necked flask of 500ml, after formula sequentially adds various raw materials more than, at room temperature, stir 1 hour.
It is made combined polyether.
The preparation of cranny filler of polyurethane foam
In 750mL inhalator jars, combined polyether 300g, polymethylene multi-phenenyl isocyanate 240g are added, then in gas Filling dimethyl ether 60g on mist agent bottle placer, the third butane 75g, shake 3min, 24h is placed at room temperature and is got product.
The single-component cranny filler of polyurethane foam made draws a design one step foaming amount for 98.8%；Get foam 4cm wide, 3cm is high, and linear meter is 33.8 meters long, is shown in Table 1.
Embodiment 3
Synthesis composite catalyst
Equipped with constant temperature water bath apparatus, and equipped with thermometer, dropping funel, churned mechanically 200ml there-necked flasks in, plus Enter 65.6 grams of 2 methyl caproic acids, open stirring.In dropping funel, 1,8- diazabicylos-bicyclic (5,4,0) -7- ten is added One 77 grams of alkene, in the case where 12 DEG C of temperature is controlled, is slowly added dropwise in there-necked flask, and drop finishes within 33 minutes.93 DEG C are warming up to, reaction 2.5 is small Shi Hou, is cooled to room temperature, filtering, obtains composite catalyst.
The preparation of combined polyether
Formula：
In the there-necked flask of 500ml, after formula sequentially adds various raw materials more than, at room temperature, stir 1 hour.
It is made combined polyether.
The preparation of cranny filler of polyurethane foam
In 750mL inhalator jars, combined polyether 300g, polymethylene multi-phenenyl isocyanate 240g are added, then in gas On mist agent bottle placer, sealing, filling dimethyl ether 60g, the third butane 75g shake 3min, 24h is placed at room temperature and is got product.
The single-component cranny filler of polyurethane foam made draws a design one step foaming amount for 98.2%；Get foam 4cm wide, 3cm is high, and linear meter is 34 meters long, is shown in Table 1.
Plain edition single-component cranny filler of polyurethane foam and case study on implementation data result of the present invention contrast statistical form table 1
Product type Surface drying speed (minute) One step foaming degree (%) Linear meter (rice/tank)
It is traditional 7 30 20.5
Embodiment 1 4 96 32.8
Embodiment 2 4 98.1 34.0
Embodiment 3 4 100 33.4

Claims (1)

1. a kind of preparation method of single-component cranny filler of polyurethane foam, it is characterized in that the preparation including composite catalyst, combination The preparation of polyethers and the preparation of cranny filler of polyurethane foam,
The preparation of composite catalyst
Formula：
Composition specification weight ratio
2 methyl caproic acid technical grade 60-80 g
1,8- diazabicylo-bicyclic (5,4,0) -7- hendecene technical grade 70-80 g
Preparation method
2 methyl caproic acid is proportionally added into there-necked flask, stirring is opened, 1,8- diazas two are being added dropwise at 10-15 DEG C of temperature Ring-bicyclic (5,4,0) -7- hendecenes, time for adding 25~35 minutes is warming up to 85~95 DEG C, and the reaction time 1.5~2.5 is small When, room temperature is down to, filter, composite catalyst is obtained,
The preparation of combined polyether
Formula：
Preparation method
In there-necked flask, after formula sequentially adds various raw materials more than, it is stirred at room temperature 1 hour, is made combined polyether,
The preparation of cranny filler of polyurethane foam
Technical formula
Preparation method
Combined polyether, polymethylene multi-phenenyl isocyanate, dimethyl ether, the third butane that will be made by formula rate, in bottle placer It is upper filling into single-component cranny filler of polyurethane foam finished product.
CN201410773472.0A 2014-12-03 2014-12-03 A kind of preparation method of single-component cranny filler of polyurethane foam Active CN104513352B (en)

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Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105733680B (en) * 2016-04-27 2017-07-14 石家庄东翔化工有限公司 Sizing paraffin preparation method for cranny filler of polyurethane foam
CN105906774A (en) * 2016-06-09 2016-08-31 营口天元化工研究所股份有限公司 Recoverable one-component polyurethane foam joint mixture contained in pressure steel cylinder
CN108865042A (en) * 2017-05-15 2018-11-23 山东居欢新型材料科技有限公司 A kind of B1 grades of flame retardant type single-component cranny filler of polyurethane foam and preparation method thereof
CN108084480A (en) * 2017-12-14 2018-05-29 安徽威朗化工科技有限公司 A kind of combined polyether and its single-component cranny filler of polyurethane foam of production
CN107880239A (en) * 2017-12-14 2018-04-06 安徽威朗化工科技有限公司 A kind of single-component cranny filler of polyurethane foam
CN109749040A (en) * 2018-12-20 2019-05-14 东元科技有限公司 A kind of single-component cranny filler of polyurethane foam
CN110183606A (en) * 2019-05-31 2019-08-30 李学友 A kind of mono-component polyurethane micro-foaming material and method with strong adhesive property
CN114478982B (en) * 2022-03-03 2023-06-09 西安科技大学 Liquid retarding hole sealing material and preparation method thereof

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CN101067072A (en) * 2007-06-05 2007-11-07 任洪青 Sealing agent of single component polyurethane foam
CN103834345A (en) * 2012-11-22 2014-06-04 湖北回天胶业股份有限公司 One-component moisture-cured polyurethane sealant with excellent ultraviolet resistance
CN104744668A (en) * 2013-12-31 2015-07-01 锋泾（中国）建材集团有限公司 Low temperature-resistant single-component polyurethane foam joint mixture and preparation method thereof

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EP2438102B1 (en) * 2009-06-05 2013-05-01 Basf Se Composites which contain a thermoformable polyurethane rigid foam, adhesive and coating material.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101067072A (en) * 2007-06-05 2007-11-07 任洪青 Sealing agent of single component polyurethane foam
CN103834345A (en) * 2012-11-22 2014-06-04 湖北回天胶业股份有限公司 One-component moisture-cured polyurethane sealant with excellent ultraviolet resistance
CN104744668A (en) * 2013-12-31 2015-07-01 锋泾（中国）建材集团有限公司 Low temperature-resistant single-component polyurethane foam joint mixture and preparation method thereof

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