CN107916088A - A kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof - Google Patents
A kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof Download PDFInfo
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- CN107916088A CN107916088A CN201711082660.9A CN201711082660A CN107916088A CN 107916088 A CN107916088 A CN 107916088A CN 201711082660 A CN201711082660 A CN 201711082660A CN 107916088 A CN107916088 A CN 107916088A
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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
- C09J175/08—Polyurethanes from polyethers
-
- 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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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
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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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
- 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
- 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
- C09J175/06—Polyurethanes from polyesters
-
- 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
- C08G2170/00—Compositions for adhesives
- C08G2170/20—Compositions for hot melt adhesives
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
Abstract
The present invention discloses a kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof, particularly a kind of suitable for moisture-curable polyurethane hot melt adhesive of PVC composite floor boards detail analysis bonding and preparation method thereof.The present invention is mainly by designing raw material proportioning and corresponding preparation process technique, so that the moisture-curable polyurethane hot melt adhesive product as obtained by prepared by the present invention more meets the bonding requirements of PVA composite floor boards, there is preferable adhesive effect to hard and soft PVC composite floor boards, and do not interfere with other performances of PVC composite floor boards.
Description
Technical field
It is particularly a kind of to be suitable in PVC floor the present invention relates to a kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof
Moisture-curable polyurethane hot melt adhesive of portion's bonding and preparation method thereof.
Background technology
Moisture-curable polyurethane hot melt adhesive is a kind of polyurethane adhesive containing end-NCO group.In use, heating melting is applied
Glue, after glue-line cooling physical solidification produces preliminary bonding force, end NCO in glue-line again with the moisture or adherend in air
The active hydrogen compounds reaction on surface, produces chemical crosslinking cure.Moisture-curable polyurethane hot melt adhesive not only has conventional thermoplastic
The positioning of hot melt adhesive rapid link, provide higher initial adhesive strength advantage, also can further cure crosslinking, make glue-line bonding force,
Cohesive strength etc. can be significantly improved.
PVC floor is a kind of home decoration composite floor board emerging in recent years, it is generally mainly by wearing layer, cushion
Bonded more with adhesive between cushion and basic unit based on PVC and mountain flour with sandwich construction composition, materials such as basic units.
At present, conventional PVC floor is bonded using solvent-based adhesive more, but the VOC content of solvent-based adhesive is generally higher,
Environmental pollution is larger and harmful.As people pay attention to the gradual of environmental protection, moisture-curable polyurethane hot melt adhesive is due to it
Body many characteristics relatively safer environmentally friendly and easy for construction etc., start in PVC composite floor field applications.
However, conventional moisture-curable polyurethane hot melt adhesive in PVC composite floor fields in application, usually in adhesive effect side
Face is performed poor, it, usually there is a phenomenon where interfacial failure, causes PVC composite floor boards whole in the experimental test of adhesive property
Body is unqualified, which bites to be solved.
The content of the invention
The purpose of the present invention, is to solve above-mentioned technical problem, there is provided a kind of moisture-curable polyurethane hot melt adhesive and its preparation
Method so that the moisture-curable polyurethane hot melt adhesive product as obtained by prepared by the present invention effectively meets material inside PVC composite floor boards
The level bonding requirements of material.
The technical solution adopted in the present invention is：A kind of moisture-curable polyurethane hot melt adhesive, its raw material is formed, by quality percentage
Than meter, including：Polyether polyol 30% ~ 50%；Polyester polyol 15% ~ 30%；Tackifying resin 5% ~ 20%；Antioxidant 0.5% ~ 1.5%；
Isocyanates 10% ~ 25%；Catalyst 0.01% ~ 0.1%；Chain extender 0.5% ~ 1.5%；Silane coupling agent 1% ~ 2%；Inorganic filler 0.5%
~1%；Plasticizer extracts agent 0.5% ~ 2% out.
Above-mentioned polyether polyol is polyoxypropyleneglycol, its number-average molecular weight is 800 ~ 2000；Preferred number average molecular weight
For 1000 polyoxypropyleneglycol.
Above-mentioned polyester polyol is selected from tetramethylene adipate glycol, adipic acid hexylene glycol esterdiol or phthalic acid fourth
The one or two of glycol esterdiol, its number-average molecular weight are 1000 ~ 4000；It is preferred that in mass ratio 1:1 configuration adipic acid oneself
The mixed material of glycol esterdiol and phthalic acid butyl glycol ester diol.
Above-mentioned tackifying resin is acrylic resin；The trade mark of antioxidant is 1010；Isocyanates is different for diphenyl methane two
Cyanate；Catalyst is stannous octoate；Chain extender is 1,4- butanediols；Silane coupling agent is γ-(the third oxygen of 2,3- epoxies) propyl group
Trimethoxy silane；Inorganic filler is nano-calcium carbonate or meteorological silica；
Above-mentioned plasticizer extracts agent out to be 7 by mass ratio:9:3:1 neopelex, saltcake, sodium tripolyphosphate and coconut palm
The mixed liquor of oily glycollic amide configuration.Meanwhile plasticizer extraction agent additive amount it is too little or too much, can influence adhesive effect or
Other performances of PVC composite floor boards in itself.
A kind of preparation method of moisture-curable polyurethane hot melt adhesive, is configured to the raw material of above-mentioned moisture-curable polyurethane hot melt adhesive
Basis, includes the following steps：
（1）Polyether polyol, polyester polyol, tackifying resin and antioxidant are proportionally added into reaction kettle and stirred, is heated
100 ~ 140 DEG C are warming up to, 2 ~ 3h is dehydrated under conditions of vacuum ＜ 200Pa；
（2）60 ~ 84 DEG C are cooled to, adds isocyanates and catalyst, stirring, under the conditions of 85 ~ 100 DEG C, vacuum ＜ 200Pa
React 60 ~ 80min；
（3）Add chain extender, the reaction was continued 40 ~ 60min；
（4）Silane coupling agent is added, stirs 0.5 ~ 1h；
（5）Inorganic filler is added, 0.5 ~ 1h is stirred under the conditions of 100 ~ 120 DEG C；
（6）Plasticizer extraction agent is added, continues 0.5 ~ 1h of stirring；
（7）Reaction terminates, and keeping drop temperature, the lower quickly discharging of nitrogen protection packs at 85-100 DEG C.
Beneficial effect of the present invention is, is compared with conventional moisture-curable polyurethane hot melt adhesive product, and institute is prepared by the present invention
The moisture-curable polyurethane hot melt adhesive product obtained more meets the bonding requirements of PVA composite floor boards, compoundly to hard and soft PVC
Plate has preferable adhesive effect, and does not interfere with other performances of PVC composite floor boards.Meanwhile preparation flow of the invention is also
It is relatively easy, products obtained therefrom moderate viscosity is prepared, also facilitates constructing operation during application.
Embodiment
The present invention is expanded on further below by embodiment, but is not intended to limit the present invention.
Embodiment 1：
A kind of moisture-curable polyurethane hot melt adhesive, raw material are formed by mass percentage, including：Polyoxypropyleneglycol 40%（Number is equal
Molecular weight 800）, tetramethylene adipate glycol 20%（Number-average molecular weight 1000）, acrylic resin 14.99%, antioxidant 0.5%,
Methyl diphenylene diisocyanate 20%, stannous octoate 0.01%, 1,4- butanediols 1%, γ-(the third oxygen of 2,3- epoxies) propyl group front three
Oxysilane 1.5%, aerosil 0.5%, and by mass ratio be 7:9:3:1 neopelex, saltcake, three
The plasticizer extraction agent 1.5% that polyphosphate sodium and the mixed liquor of cocounut oil glycollic amide configuration are formed.
The preparation method of above-mentioned moisture-curable polyurethane hot melt adhesive, step are as follows：
（1）Polyoxypropyleneglycol, tetramethylene adipate glycol, acrylic resin and antioxidant are added in reaction kettle and stirred
Mix uniformly, be heated to 130 DEG C, 2h is dehydrated under conditions of vacuum ＜ 200Pa；
（2）It is cooled to 76 DEG C, adds methyl diphenylene diisocyanate and stannous octoate, stirring, at 85 DEG C, vacuum 180Pa
Under the conditions of react 70min；
（3）Add 1,4-butanediol, the reaction was continued 50min；
（4）γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added, stirs 1h；
（5）Aerosil is added, 0.5h is stirred under the conditions of 120 DEG C；
（6）It is 7 to add by mass ratio:9:3:1 neopelex, saltcake, sodium tripolyphosphate and cocounut oil glycollic amide
The plasticizer extraction agent that the mixed liquor of configuration is formed, continues to stir 0.5h；
（7）Reaction terminates, and keeping drop temperature, the lower quickly discharging of nitrogen protection packs at 90 DEG C.
A1 is labeled as according to 1 products therefrom sample of embodiment.
Embodiment 2：
A kind of moisture-curable polyurethane hot melt adhesive, raw material are formed according to the mass fraction, including：Polyoxypropyleneglycol 31.9%（Number is equal
Molecular weight 1000）, adipic acid hexylene glycol esterdiol 30%（Number-average molecular weight 2000）, acrylic resin 20%, antioxidant 1.5%, two
Methylenebis phenyl isocyanate 10%, stannous octoate 0.1%, 1,4- butanediols 1.5%, γ-(the third oxygen of 2,3- epoxies) propyl group front three
Oxysilane 2%, nano-calcium carbonate 1%, and by mass ratio be 7:9:3:1 neopelex, saltcake, tripolyphosphate
The plasticizer extraction agent 2% that sodium and the mixed liquor of cocounut oil glycollic amide configuration are formed.
The preparation method of above-mentioned moisture-curable polyurethane hot melt adhesive, step are as follows：
（1）Polyoxypropyleneglycol, adipic acid hexylene glycol esterdiol, acrylic resin and antioxidant are added in reaction kettle and stirred
Mix uniformly, be heated to 120 DEG C, 2.5h is dehydrated under conditions of vacuum ＜ 200Pa；
（2）It is cooled to 80 DEG C, adds methyl diphenylene diisocyanate and stannous octoate, stirring, at 90 DEG C, vacuum 180Pa
Under the conditions of react 60min；
（3）Add 1,4-butanediol, the reaction was continued 40min；
（4）γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added, stirs 0.5h；
（5）Nano-calcium carbonate is added, 0.5h is stirred under the conditions of 110 DEG C；
（6）It is 7 to add by mass ratio:9:3:1 neopelex, saltcake, sodium tripolyphosphate and cocounut oil glycollic amide
The plasticizer extraction agent that the mixed liquor of configuration is formed, continues to stir 1h；
（7）Reaction terminates, and keeping drop temperature, the lower quickly discharging of nitrogen protection packs at 95 DEG C.
A2 is labeled as according to 2 products therefrom sample of embodiment.
Embodiment 3
A kind of moisture-curable polyurethane hot melt adhesive, raw material are formed according to the mass fraction, including：Polyoxypropyleneglycol 45%（Number is divided equally
Son amount 1500）, tetramethylene adipate glycol 10%（Number-average molecular weight 3000）, phthalic acid butyl glycol ester diol 10% (number
Average molecular weight 3000), acrylic resin 5%, antioxidant 1%, methyl diphenylene diisocyanate 25%, stannous octoate 0.1%, 1,4-
Butanediol 0.5%, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane 1%, aerosil 1%, and be by mass ratio
7:9:3:The plasticising that the mixed liquor that 1 neopelex, saltcake, sodium tripolyphosphate and cocounut oil glycollic amide configures is formed
Agent 1.4% is extracted in agent out.
The preparation method of above-mentioned moisture-curable polyurethane hot melt adhesive, step are as follows：
（1）By polyoxypropyleneglycol, tetramethylene adipate glycol, phthalic acid butyl glycol ester diol, acrylic resin
It is added in reaction kettle and stirs evenly with antioxidant, be heated to 130 DEG C, 3h is dehydrated under conditions of vacuum ＜ 200Pa；
（2）It is cooled to 76 DEG C, adds methyl diphenylene diisocyanate and stannous octoate, stirring, at 85 DEG C, vacuum 180Pa
Under the conditions of react 80min；
（3）Add 1,4-butanediol, the reaction was continued 60min；
（4）γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added, stirs 1h；
（5）Aerosil is added, 1h is stirred under the conditions of 120 DEG C；
（6）It is 7 to add by mass ratio:9:3:1 neopelex, saltcake, sodium tripolyphosphate and cocounut oil glycollic amide
The plasticizer extraction agent that the mixed liquor of configuration is formed, continues to stir 1h；
（7）Reaction terminates, and keeping drop temperature, the lower quickly discharging of nitrogen protection packs at 90 DEG C.
A3 is labeled as according to 3 products therefrom sample of embodiment.
Embodiment 4
A kind of moisture-curable polyurethane hot melt adhesive, raw material are formed according to the mass fraction, including：Polyoxypropyleneglycol 50%（Number is divided equally
Son amount 2000）, phthalic acid butyl glycol ester diol 15% (number-average molecular weight 4000), acrylic resin 15%, antioxidant 1%, two
Methylenebis phenyl isocyanate 15%, stannous octoate 0.1%, 1,4- butanediols 1.4%, γ-(the third oxygen of 2,3- epoxies) propyl group front three
Oxysilane 1%, aerosil 1%, and by mass ratio be 7:9:3:1 neopelex, saltcake, trimerization phosphorus
The plasticizer extraction agent 0.5% that the mixed liquor of sour sodium and cocounut oil glycollic amide configuration is formed.
The preparation method of above-mentioned moisture-curable polyurethane hot melt adhesive, step are as follows：
（1）Polyoxypropyleneglycol, phthalic acid butyl glycol ester diol, acrylic resin and antioxidant are added to reaction kettle
In stir evenly, be heated to 110 DEG C, 2h be dehydrated under conditions of vacuum ＜ 200Pa；
（2）It is cooled to 76 DEG C, adds methyl diphenylene diisocyanate and stannous octoate, stirring, at 85 DEG C, vacuum 180Pa
Under the conditions of react 70min；
（3）Add 1,4-butanediol, the reaction was continued 50min；
（4）γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added, stirs 1h；
（5）Aerosil is added, 0.5h is stirred under the conditions of 120 DEG C；
（6）It is 7 to add by mass ratio:9:3:1 neopelex, saltcake, sodium tripolyphosphate and cocounut oil glycollic amide
The plasticizer extraction agent that the mixed liquor of configuration is formed, continues to stir 0.5h；
（7）Reaction terminates, and keeping drop temperature, the lower quickly discharging of nitrogen protection packs at 90 DEG C.
A4 is labeled as according to 4 products therefrom sample of embodiment.
By above-mentioned each Product samples A1 ~ A4 and commercially available conventional moisture-curable polyurethane hot melt adhesive D1 compoundly applied to PVC
Plate, and carry out correlated performance detection.Viscosity testing standard refers to GB/T 2794, and the testing standard of peel strength refers to GB/T
7122, test result is as shown in table 1 below.
Claims (6)
1. a kind of moisture-curable polyurethane hot melt adhesive, it is characterised in that the raw material of the moisture-curable polyurethane hot melt adhesive is formed, by matter
Percentages are measured, including：
Polyether polyol 30% ~ 50%；
Polyester polyol 15% ~ 30%；
Tackifying resin 5% ~ 20%；
Antioxidant 0.5% ~ 1.5%；
Isocyanates 10% ~ 25%；
Catalyst 0.01% ~ 0.1%；
Chain extender 0.5% ~ 1.5%；
Silane coupling agent 1% ~ 2%；
Inorganic filler 0.5% ~ 1%；
Plasticizer extracts agent 0.5% ~ 2% out；
The plasticizer extracts agent out by four kinds of neopelex, saltcake, sodium tripolyphosphate and cocounut oil glycollic amide materials
Mixed configuration forms, and neopelex, saltcake, the mass ratio of sodium tripolyphosphate and cocounut oil glycollic amide are 7:9:3:
1。
2. moisture-curable polyurethane hot melt adhesive as claimed in claim 1, it is characterised in that：The polyether polyol is polyoxygenated third
Enediol, its number-average molecular weight are 800 ~ 2000；The number-average molecular weight of the polyester polyol be 1000 ~ 4000, select oneself two
The one or two of sour butyl glycol ester diol, adipic acid hexylene glycol esterdiol or phthalic acid butyl glycol ester diol；The increasing
Viscosity resin is acrylic resin；The trade mark of the antioxidant is 1010；The isocyanates is methyl diphenylene diisocyanate；
The catalyst is stannous octoate；The chain extender is 1,4- butanediols；The silane coupling agent is γ-(the third oxygen of 2,3- epoxies)
Propyl trimethoxy silicane；The inorganic filler is nano-calcium carbonate or meteorological silica.
3. moisture-curable polyurethane hot melt adhesive as claimed in claim 2, it is characterised in that：The number of the polyoxypropyleneglycol is equal
Molecular weight is 1000.
4. moisture-curable polyurethane hot melt adhesive as claimed in claim 2, it is characterised in that：The polyester polyol for adipic acid oneself
The mixed material of glycol esterdiol and phthalic acid butyl glycol ester diol.
5. moisture-curable polyurethane hot melt adhesive as claimed in claim 4, it is characterised in that：The adipic acid hexylene glycol esterdiol and
The mass ratio of phthalic acid butyl glycol ester diol is 1:1.
6. a kind of preparation method of moisture-curable polyurethane hot melt adhesive, it is characterised in that with the described wet solid of above-mentioned 1 to 5 any one
On the basis of the raw material composition for changing polyurethane hot melt, preparation process is as follows：
（1）Polyether polyol, polyester polyol, tackifying resin and antioxidant are proportionally added into reaction kettle and stirred, is heated
100 ~ 140 DEG C are warming up to, 2 ~ 3h is dehydrated under conditions of vacuum ＜ 200Pa；
（2）60 ~ 84 DEG C are cooled to, adds isocyanates and catalyst, stirring, under the conditions of 85 ~ 100 DEG C, vacuum ＜ 200Pa
React 60 ~ 80min；
（3）Add chain extender, the reaction was continued 40 ~ 60min；
（4）Silane coupling agent is added, stirs 0.5 ~ 1h；
（5）Inorganic filler is added, 0.5 ~ 1h is stirred under the conditions of 100 ~ 120 DEG C；
（6）Plasticizer extraction agent is added, continues 0.5 ~ 1h of stirring；
（7）Reaction terminates, and keeping drop temperature, the lower quickly discharging of nitrogen protection packs at 85-100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711082660.9A CN107916088A (en) | 2017-11-07 | 2017-11-07 | A kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711082660.9A CN107916088A (en) | 2017-11-07 | 2017-11-07 | A kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof |
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|---|---|
| CN107916088A true CN107916088A (en) | 2018-04-17 |
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| CN201711082660.9A Pending CN107916088A (en) | 2017-11-07 | 2017-11-07 | A kind of moisture-curable polyurethane hot melt adhesive and preparation method thereof |
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| CN109321191A (en) * | 2018-08-22 | 2019-02-12 | 上海天洋热熔粘接材料股份有限公司 | A kind of preparation method of moisture-curable polyurethane hot melt adhesive |
| CN110283291A (en) * | 2019-06-11 | 2019-09-27 | 南通天洋新材料有限公司 | A kind of modified moisture-curable polyurethane hot melt adhesive and preparation method thereof |
| CN111040127A (en) * | 2019-12-28 | 2020-04-21 | 海隆石油产品技术服务（上海）有限公司 | Hot melt adhesive for stone plastic floor and preparation method thereof |
| CN111205804A (en) * | 2020-03-12 | 2020-05-29 | 烟台德邦科技有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method thereof |
| CN111909650A (en) * | 2020-07-03 | 2020-11-10 | 江苏龙蟠科技股份有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method thereof |
| CN112391141A (en) * | 2020-11-06 | 2021-02-23 | 广东泰强化工实业有限公司 | Nano silicon dioxide polyurethane hot melt adhesive and preparation method thereof |
| CN114989765A (en) * | 2021-03-01 | 2022-09-02 | 深圳科创新源新材料股份有限公司 | Thermoplastic underfill material and preparation method and application thereof |
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| CN109321191A (en) * | 2018-08-22 | 2019-02-12 | 上海天洋热熔粘接材料股份有限公司 | A kind of preparation method of moisture-curable polyurethane hot melt adhesive |
| CN110283291A (en) * | 2019-06-11 | 2019-09-27 | 南通天洋新材料有限公司 | A kind of modified moisture-curable polyurethane hot melt adhesive and preparation method thereof |
| CN111040127A (en) * | 2019-12-28 | 2020-04-21 | 海隆石油产品技术服务（上海）有限公司 | Hot melt adhesive for stone plastic floor and preparation method thereof |
| CN111040127B (en) * | 2019-12-28 | 2021-10-22 | 海隆石油产品技术服务（上海）有限公司 | Hot melt adhesive for stone plastic floor and preparation method thereof |
| CN111205804A (en) * | 2020-03-12 | 2020-05-29 | 烟台德邦科技有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method thereof |
| CN111909650A (en) * | 2020-07-03 | 2020-11-10 | 江苏龙蟠科技股份有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method thereof |
| CN112391141A (en) * | 2020-11-06 | 2021-02-23 | 广东泰强化工实业有限公司 | Nano silicon dioxide polyurethane hot melt adhesive and preparation method thereof |
| CN114989765A (en) * | 2021-03-01 | 2022-09-02 | 深圳科创新源新材料股份有限公司 | Thermoplastic underfill material and preparation method and application thereof |
| CN114989765B (en) * | 2021-03-01 | 2024-02-20 | 深圳科创新源新材料股份有限公司 | Thermoplastic underfill material, and preparation method and application thereof |
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