CN107011853A - A kind of quick-setting polyurethane hot melt and preparation method thereof - Google Patents

A kind of quick-setting polyurethane hot melt and preparation method thereof Download PDF

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Publication number
CN107011853A
CN107011853A CN201710400656.6A CN201710400656A CN107011853A CN 107011853 A CN107011853 A CN 107011853A CN 201710400656 A CN201710400656 A CN 201710400656A CN 107011853 A CN107011853 A CN 107011853A
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poly
hot melt
polyurethane hot
quick
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陈庆玲
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Yantai Zhiben Intellectual Property Operation and Management Co Ltd
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Yantai Zhiben Intellectual Property Operation and Management Co Ltd
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Priority to CN201710400656.6A priority Critical patent/CN107011853A/en
Publication of CN107011853A publication Critical patent/CN107011853A/en
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    • 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
    • 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
    • C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
    • C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
    • C08G18/4211—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
    • 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
    • C08G18/4825—Polyethers containing two hydroxy groups
    • 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
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/69—Polymers of conjugated dienes
    • C08G18/692—Polymers of conjugated dienes containing carboxylic acid groups
    • 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
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/544—Silicon-containing compounds containing nitrogen
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention belongs to high polymer material and its preparing technical field, more particularly to a kind of quick-setting polyurethane hot melt and preparation method thereof.Polyoxypropyleneglycol, the poly- phthalic acid hexylene glycol esterdiol of the present invention is mixed with poly methylene poly phenyl poly isocyanate, improves the solidification effect of PUR；Dibutyl tin laurate can avoid heating the foaming phenomena after adhesive curing, improve the outward appearance after its solidification；KH550 consumption is improved, the bonding force of PUR is improved, while bonding force is improved, and toxic raw material is not introduced into, does not also influence the storage period of PUR；Using higher-strength can be obtained after 4 6h, technique interval time is substantially reduced, it is cost-effective while improving process efficiency.

Description

A kind of quick-setting polyurethane hot melt and preparation method thereof
Technical field
The invention belongs to high polymer material and its preparing technical field, more particularly to a kind of quick-setting polyurethane-hot melt Glue and preparation method thereof.
Background technology
Polyurethane is a kind of high polymer material.Being widely used such as the paint and coating in furniture, family in daily life Roof water-proof heat-insulation layer and coating for internal and external wall in refrigerator and refrigerator in electrical appliance, construction industry etc..It can be made into various poly- Urethane material such as polyurethane shoe-sole, polyurethane fiber, polyurethane sealant etc..Polyurethane product performance adjustable extent on the whole Width, strong adaptability, resistance to biological aging, moderate cost, are widely used in numerous industries such as upholstery, construction industry, transportation industry.
Polyurethane-hot melt adhesive curing is slower, generally requires to wait after the long period (general cold curing 7 days) just after construction Next step operation can be carried out, causes construction technology to extend, is unfavorable for the saving of production cost and the raising of process efficiency.
The content of the invention
There is provided a kind of quick-setting polyurethane hot melt and its system for deficiency of the invention for the presence of above-mentioned prior art Preparation Method.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：A kind of quick-setting polyurethane hot melt, by with Each component composition of lower parts by weight：20-25 parts of polyoxypropyleneglycols, 15-40 parts of poly- phthalic acid hexylene glycol esters two Alcohol, 8-15 part dioctyl phthalate, 5-8 parts of CTPB liquid rubbers, 2.5-4 parts of polymethylene polyphenyls are more Isocyanates, 1-3 part lead octoate, 1.5-2.8 parts of triethylamines, 5-6 parts of ball-shaped silicon micro powders, the 0.04-0.08 parts of fourths of tin dilaurate two Ji Xi and 0.3-0.6 parts of KH550.
Preferably, it is made up of each component of following parts by weight：23 parts of polyoxypropyleneglycols, 40 parts of poly- O-phthalics Sour hexylene glycol esterdiol, 10 parts of dioctyl phthalates, 8 parts of CTPB liquid rubbers, 2.5 parts of polymethylenes are more Polyphenyl polyisocyanate, 2 parts of lead octoates, 1.5 parts of triethylamines, 5.5 parts of ball-shaped silicon micro powders, 0.04 part of dibutyl tin laurate and 0.6 part of KH550.
The preparation method of above-mentioned quick-setting polyurethane hot melt, step is as follows：
(1) 20-25 parts polyoxypropyleneglycol, the 15-40 parts of poly- O-phthalics of dewater treatment are added into reactor Sour hexylene glycol esterdiol, 8-15 parts of dioctyl phthalates, 5-8 parts of CTPB liquid rubbers and 2.5-4 parts are more Polymethylene polyphenyl polyisocyanates, is stirred under vacuum 30min；
(2) by pre-dry 1-3 parts of lead octoate, 1.5-2.8 parts of triethylamines and 5-6 parts of ball-shaped silicon micro powders, input reaction In kettle, 30min is stirred under vacuum；,
(3) finally, 0.04-0.08 parts of dibutyl tin laurates and 0.3-0.6 parts of KH550 are added into reactor, are filled Divide after stirring 30min, produce quick-setting polyurethane hot melt.
The beneficial effects of the invention are as follows：The present invention polyoxypropyleneglycol, poly- phthalic acid hexylene glycol esterdiol with Poly methylene poly phenyl poly isocyanate is mixed, and improves the solidification effect of PUR；Dibutyl tin laurate can avoid heat Foaming phenomena after melten gel solidification, improves the outward appearance after its solidification；KH550 consumption is improved, the bonding force of PUR is improved, While bonding force is improved, and toxic raw material is not introduced into, does not also influence the storage period of PUR；It is using after 4-6h Higher-strength can be obtained, technique interval time is substantially reduced, it is cost-effective while improving process efficiency.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit Determine the scope of the present invention.
Embodiment 1
A kind of quick-setting polyurethane hot melt, is made up of each component of following parts by weight：23 parts of polyoxygenateds third Enediol, 40 parts of poly- phthalic acid hexylene glycol esterdiols, 10 parts of dioctyl phthalates, 8 parts of CTPB liquid Body rubber, 2.5 parts of poly methylene poly phenyl poly isocyanates, 2 parts of lead octoates, 1.5 parts of triethylamines, 5.5 parts of ball-shaped silicon micro powders, 0.04 part of dibutyl tin laurate and 0.6 part of KH550.
The preparation method of above-mentioned quick-setting polyurethane hot melt, step is as follows：
(1) added into reactor 23 parts of polyoxypropyleneglycols of dewater treatment, 40 parts of poly- phthalic acids oneself two Alcohol esterdiol, 10 parts of dioctyl phthalates, 8 parts of CTPB liquid rubbers and 2.5 parts of polymethylene polyphenyls Polyisocyanates, is stirred under vacuum 30min；
(2) by pre-dry 2 parts of lead octoates, 1.5 parts of triethylamines and 5.5 parts of ball-shaped silicon micro powders, in input reactor, very Sky stirring 30min；,
(3) finally, 0.04 part of dibutyl tin laurate and 0.6 part of KH550 are added into reactor, is sufficiently stirred for After 30min, quick-setting polyurethane hot melt is produced.
Embodiment 2
A kind of quick-setting polyurethane hot melt, is made up of each component of following parts by weight：20 parts of polyoxygenateds third Enediol, 15 parts of poly- phthalic acid hexylene glycol esterdiols, 15 parts of dioctyl phthalates, 5 parts of CTPB liquid Body rubber, 4 parts of poly methylene poly phenyl poly isocyanates, 1 part of lead octoate, 2.8 parts of triethylamines, 5 parts of ball-shaped silicon micro powders, 0.08 part Dibutyl tin laurate and 0.3 part of KH550.
The preparation method of above-mentioned quick-setting polyurethane hot melt, step is as follows：
(1) added into reactor 20 parts of polyoxypropyleneglycols of dewater treatment, 15 parts of poly- phthalic acids oneself two Alcohol esterdiol, 15 parts of dioctyl phthalates, 5 parts of CTPB liquid rubbers and 4 parts of polymethylene polyphenyls are more Isocyanates, is stirred under vacuum 30min；
(2) by pre-dry 1 part of lead octoate, 2.8 parts of triethylamines and 5 parts of ball-shaped silicon micro powders, in input reactor, vacuum Stir 30min；,
(3) finally, 0.08 part of dibutyl tin laurate and 0.3 part of KH550 are added into reactor, is sufficiently stirred for After 30min, quick-setting polyurethane hot melt is produced.
Comparative example
A kind of preparation method of polyurethane hot melt, step is as follows：
(1) polyoxypropyleneglycol that the PPOX triol 150kg for being 5000 by molecular weight, molecular weight are 4000 120kg and 40kg MDI react 3h under the conditions of 85 DEG C, and it is 2.30% to measure NCO terminals, standby；
(2) precipitated calcium carbonate is removed water into 48h in 110 DEG C of baking ovens, and keeps heated condition standby；Detect plasticizer DINP Moisture, controls its water content less than 0.05%, standby；
(3) the plasticizer DINP 20kg steps of step (2) are added in the 150L planet stirring kettles for can lead to recirculated water (1) performed polymer 45kg and oxazolidine deicer 0.8kg, are evacuated to vacuum and are stirred until homogeneous for -0.095~-0.1MPa Without particle；
(4) the precipitated calcium carbonate 17kg of step (2) is added into step (3), cooling water circulation is passed through and is evacuated to vacuum Spend and be stirred until homogeneous no particle for -0.095~-0.1MPa；
(5) 0.5kg coupling agent KH560,0.10kg dibutyl tin laurates are added into step (4), are evacuated to true Reciprocal of duty cycle is that -0.095~-0.1MPa is stirred until homogeneous, and polyurethane hot melt is made.
Polyurethane hot melt prepared by polyurethane hot melt made from above-described embodiment 1-2 and comparative example is through country Standard Mechanics Performance Testing, data result is as shown in table 1.
The polyurethane sealant of table 1 and comparative example performance comparision
By the performance test table of comparisons of table 1, it can be seen that polyurethane hot melt prepared by the present invention gathers relative to conventional Urethane PUR shows excellent solidification rapid charater, using that can obtain higher-strength after 4-6h, substantially reduces technique It is interval time, cost-effective while improve process efficiency and poly- better than common in terms of tensile strength and shear strength Urethane PUR.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (3)

1. a kind of quick-setting polyurethane hot melt, it is characterised in that be made up of each component of following parts by weight：20- 25 parts of polyoxypropyleneglycols, 15-40 parts of poly- phthalic acid hexylene glycol esterdiols, 8-15 parts of dioctyl phthalates, 5-8 Part CTPB liquid rubber, 2.5-4 parts of poly methylene poly phenyl poly isocyanates, 1-3 parts of lead octoates, 1.5-2.8 Part triethylamine, 5-6 parts of ball-shaped silicon micro powders, 0.04-0.08 parts of dibutyl tin laurates and 0.3-0.6 parts of KH550.
2. polyurethane hot melt according to claim 1, it is characterised in that by each component group of following parts by weight Into：23 parts of polyoxypropyleneglycols, 40 parts of poly- phthalic acid hexylene glycol esterdiols, 10 parts of dioctyl phthalates, 8 parts of ends CTPB, 2.5 parts of poly methylene poly phenyl poly isocyanates, 2 parts of lead octoates, 1.5 parts of triethylamines, 5.5 Part ball-shaped silicon micro powder, 0.04 part of dibutyl tin laurate and 0.6 part of KH550.
3. the preparation method of quick-setting polyurethane hot melt described in a kind of claim 1 or 2, it is characterised in that step is such as Under：
(1) added into reactor 20-25 parts polyoxypropyleneglycol of dewater treatment, 15-40 parts of poly- phthalic acids oneself Glycol esterdiol, 8-15 part dioctyl phthalate, 5-8 parts of CTPB liquid rubbers and 2.5-4 parts of many methylenes Quito polyphenyl polyisocyanate, is stirred under vacuum 30min；
(2) by pre-dry 1-3 parts of lead octoate, 1.5-2.8 parts of triethylamines and 5-6 parts of ball-shaped silicon micro powders, in input reactor, It is stirred under vacuum 30min；,
(3) finally, 0.04-0.08 parts of dibutyl tin laurates and 0.3-0.6 parts of KH550 are added into reactor, are fully stirred Mix after 30min, produce quick-setting polyurethane hot melt.
CN201710400656.6A 2017-05-31 2017-05-31 A kind of quick-setting polyurethane hot melt and preparation method thereof Withdrawn CN107011853A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110655893A (en) * 2019-08-28 2020-01-07 苏州德圣辉新能源科技有限公司 High-strength repair adhesive for solar backboard and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102477274A (en) * 2010-11-26 2012-05-30 上海恩意材料科技有限公司 Polyurethane thermosol adhesive
CN104694067A (en) * 2015-02-16 2015-06-10 济南汉斯曼时代技术有限公司 Rapid-curing high-strength bi-component polyurethane bonding glue and preparation method of bonding glue
CN105255435A (en) * 2015-10-19 2016-01-20 烟台德邦科技有限公司 Preparation method of photo-moisture dual cured hot melt polyurethane sealant
CN105367736A (en) * 2015-12-01 2016-03-02 烟台德邦科技有限公司 Preparation method for polyurethane hot melt adhesive with good reworking performance

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102477274A (en) * 2010-11-26 2012-05-30 上海恩意材料科技有限公司 Polyurethane thermosol adhesive
CN104694067A (en) * 2015-02-16 2015-06-10 济南汉斯曼时代技术有限公司 Rapid-curing high-strength bi-component polyurethane bonding glue and preparation method of bonding glue
CN105255435A (en) * 2015-10-19 2016-01-20 烟台德邦科技有限公司 Preparation method of photo-moisture dual cured hot melt polyurethane sealant
CN105367736A (en) * 2015-12-01 2016-03-02 烟台德邦科技有限公司 Preparation method for polyurethane hot melt adhesive with good reworking performance

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110655893A (en) * 2019-08-28 2020-01-07 苏州德圣辉新能源科技有限公司 High-strength repair adhesive for solar backboard and preparation method thereof

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