Preparation process of two-component PUR (moisture-curing hot melt adhesive)

Abstract

The invention relates to the technical field of moisture-curing hot melt adhesives, and discloses a double-component PUR (moisture-curing hot melt adhesive) preparation process which comprises a component A and a component B. The component A is a prepolymer prepared by reacting dihydric alcohol with the molecular weight of 1000-5000 with diisocyanate, organic acid is added as a polymerization inhibitor, and proper liquid paraffin is added as a surface sealant; the component B is prepared by melting and uniformly mixing polyester polyol with the molecular weight of 1000-3000 and good crystallinity and binary polyether amine with the molecular weight of 2000-5000 at a high temperature, cooling to below 60 DEG C, adding metered diisocyanate, and controlling the R value to be 0.3-0.7. According to the preparation process of the two-component PUR (moisture-curing hot melt adhesive), a two-component process is adopted, the part A is relatively large in R, high in NCO group content and relatively large in moisture and high-temperature tolerance, and meanwhile, the stability is further improved by adding a polymerization inhibitor and a sealant; and crystals formed at low temperature of the component B can be used for quickly cleaning the pipeline through proper heating and an environment-friendly cleaning agent such as ethyl acetate, and can be repeatedly utilized.

Description

Technical Field

[0001] The invention relates to the technical field of moisture-curing hot melt adhesives, in particular to a preparation process of two-component PUR (moisture-curing hot melt adhesive). Background Art

[0002] Moisture-curing hot melt adhesive is a type of adhesive that uses moisture in the air of a humid environment to initiate curing. When moisture comes into contact with the glue, the water in the moisture causes the glue to undergo a chemical reaction, curing it into a strong adhesive. This curing method gives moisture-curing hot melt adhesives unique performance advantages.

[0003] Moisture-curing hot melt adhesives are widely used in various fields due to their excellent performance, such as the packaging industry, construction industry, and automotive industry. Traditional PUR has a low R and a low content of active NCO groups. It is easy to polymerize in an environment with high humidity or temperature and loses its hot-melt function. Therefore, during the production and storage process, strict temperature and humidity control is required. The environment and packaging materials and equipment requirements are extremely high, resulting in high production costs. Therefore, a two-component moisture-curing hot melt adhesive PUR is urgently needed. Summary of the invention

[0004] The purpose of the present invention is to provide a two-component PUR (moisture-curing hot melt adhesive) preparation process to solve the problem that the traditional PUR proposed in the above background technology has a low R, a low content of active NCO groups, is easily polymerized in an environment with high air humidity or high temperature, and loses its hot melt function. Therefore, during the production and storage process, strict temperature and humidity control, environment and packaging materials, and equipment requirements are extremely high, resulting in high production costs.

[0005] In order to solve the above technical problems, the present invention provides the following technical solution: a two-component PUR (moisture curing hot melt adhesive), comprising component A and component B, wherein:

[0006] Component A is a prepolymer prepared by reacting a diol with a molecular weight of 1000-5000 with a diisocyanate, an organic acid is added as an inhibitor, and appropriate liquid paraffin is added as a surface sealant;

[0007] Component B is prepared by melting and mixing polyester polyol with good crystallinity of molecular weight 1000-3000 and dibasic polyetheramine with molecular weight 2000-5000 at high temperature, cooling to below 60°C, adding measured diisocyanate, controlling R value between 0.3-0.7, and obtaining hydroxyl terminated resin part.

[0008] Preferably, the diol is selected from one or more of polyethylene glycol, polypropylene glycol and polytetramethylene glycol.

[0009] Preferably, the diisocyanate is selected from one or more of toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), and isophorone diisocyanate (IPDI).

[0010] Preferably, the organic acid is selected from one or more of benzoic acid, acetic acid and oxalic acid.

[0011] Preferably, the polyester polyol is selected from one or more of polyethylene adipate, polybutylene adipate, and polyethylene terephthalate.

[0012] Preferably, the divalent polyetheramine is selected from one or more of ethylenediamine, diethylenetriamine and triethylenetetramine.

[0013] Preferably, the preparation process of two-component PUR (moisture curing hot melt adhesive) comprises the following steps:

[0014] Preparation of component A: react diol with a molecular weight of 1000-5000 with diisocyanate at a certain temperature to prepare a prepolymer, then add an organic acid as an inhibitor, and then add an appropriate amount of liquid paraffin as a surface sealant, and mix well;

[0015] Preparation of component B: melt and mix polyester polyol with good crystallinity and molecular weight of 1000-3000 and dibasic polyetheramine with molecular weight of 2000-5000 at high temperature, cool to below 60°C, add measured diisocyanate, control R value between 0.3-0.7, and obtain hydroxyl-terminated resin part;

[0016] When in use, preheat component A and component B to a good fluidity state respectively, mix them thoroughly with a two-component glue gun, control the R value between 1.2-1.5, and prepare the moisture-curing hot melt adhesive PUR.

[0017] Preferably, during the preparation of component A, the reaction temperature is 80-120° C. and the reaction time is 2-4 hours.

[0018] Preferably, during the preparation of the B component, the high temperature melting temperature is 150-200°C, and the cooling rate after uniform mixing is 1-2°C / min.

[0019] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0020] First, the present invention adopts a two-component process, the R of part A is larger, the NCO group content is high, and it has a greater tolerance to moisture and high temperature. At the same time, the stability is further improved by adding inhibitors and sealants.

[0021] Second, the present invention adopts a two-component process, and the crystals formed by the low temperature of component B can be used to quickly clean the pipeline through appropriate heating and environmentally friendly cleaning agents such as ethyl acetate, and can be reused.

[0022] Second, the present invention adopts a two-component process, and the B component adopts a mixture of highly active diamines and polyester diols and polyether diols, which has a fast reaction speed, a short setting time, and a wide range of applications, and can meet the application fields of home decoration film, edge sealing, rapid installation of automobile interior decoration, clothing, etc. DETAILED DESCRIPTION

[0023] In order to better understand and implement the present invention, the technical scheme and implementation steps of the present invention are described in detail below through specific embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Embodiment 1

[0025] The two-component PUR (moisture curing hot melt adhesive) preparation process includes the following steps:

[0026] Preparation of Component A

[0027] Raw material preparation: polyethylene glycol (PEG) with molecular weight of 1000-5000: 100 g;

[0028] Methylene diphenyl diisocyanate (MDI): 200 g;

[0029] Benzoic acid: 0.5 g;

[0030] Liquid paraffin: 10 grams.

[0031] Preparation steps: 100 g of polyethylene glycol (PEG) and 200 g of diphenylmethane diisocyanate (MDI) were added to a reaction kettle, heated to 100° C., stirred and reacted for 3 hours under nitrogen protection to obtain a prepolymer;

[0032] After the reaction was completed, 0.5 g of benzoic acid was added to the reactor as a polymerization inhibitor and stirring was continued for 10 minutes;

[0033] Then add 10 g of liquid paraffin as a surface sealant, and continue stirring for 10 minutes until the mixture is evenly mixed to obtain component A.

[0034] Preparation of component B

[0035] Raw material preparation: polyethylene adipate (PBA) with a molecular weight of 1000-3000: 100 g;

[0036] Diethylenetriamine (DETA) with a molecular weight of 2000-5000: 100 g;

[0037] Methylene diphenyl diisocyanate (MDI): 50 g.

[0038] Preparation steps: add 100 g of polyethylene adipate (PBA) and 100 g of diethylenetriamine (DETA) into a reaction kettle, heat to 180° C., stir and mix evenly under nitrogen protection, and then slowly cool to 60° C.;

[0039] After cooling to 60°C, add 50 g of diphenylmethane diisocyanate (MDI), control the R value to 0.5, and continue stirring for 30 minutes until the mixture is evenly mixed to obtain component B.

[0040] How to use

[0041] Preheating: Preheat component A to 80°C and component B to 60°C to ensure that the two components have good fluidity;

[0042] Mixing: Mix the preheated component A and component B in a weight ratio of 1:1 using a two-component glue gun, and control the R value to 1.3;

[0043] Construction: Apply the mixed glue evenly on the surface of the material to be bonded and cure it at room temperature for 1-3 hours.

[0044] Embodiment 2

[0045] The two-component PUR (moisture curing hot melt adhesive) preparation process includes the following steps:

[0046] Preparation of Component A

[0047] Raw material preparation: Polypropylene glycol (PPG) with a molecular weight of 2000-3000: 120 g;

[0048] Isophorone diisocyanate (IPDI): 240 g;

[0049] Acetic acid: 0.6 g;

[0050] Liquid paraffin: 12 g.

[0051] Preparation steps: 120 g of polypropylene glycol (PPG) and 240 g of isophorone diisocyanate (IPDI) were added into a reaction kettle, heated to 110° C., stirred and reacted for 3 hours under nitrogen protection to obtain a prepolymer;

[0052] After the reaction was completed, 0.6 g of acetic acid was added to the reactor as a polymerization inhibitor and stirring was continued for 10 minutes;

[0053] Then add 12 grams of liquid paraffin as a surface sealant, and continue stirring for 10 minutes until the mixture is uniformly mixed to obtain component A.

[0054] Preparation of component B

[0055] Raw material preparation: Polybutylene adipate (PBD) with a molecular weight of 1500-2500: 120 g;

[0056] Triethylenetetramine (TETA) with a molecular weight of 3000-4000: 120 g;

[0057] Methylene diphenyl diisocyanate (MDI): 60 g.

[0058] Preparation steps: 120 g of polybutylene adipate (PBD) and 120 g of triethylenetetramine (TETA) were added to a reaction kettle, heated to 180° C., stirred and mixed evenly under nitrogen protection, and then slowly cooled to 60° C.;

[0059] After cooling to 60°C, add 60 g of diphenylmethane diisocyanate (MDI), control the R value to 0.5, and continue stirring for 30 minutes until the mixture is evenly mixed to obtain component B.

[0060] How to use

[0061] Preheating: Preheat component A to 90°C and component B to 70°C to ensure that both components have good fluidity;

[0062] Mixing: Mix the preheated component A and component B thoroughly in a weight ratio of 1:1.2 using a two-component glue gun, and control the R value to 1.4;

[0063] Construction: Apply the mixed glue evenly on the surface of the material to be bonded and cure it at room temperature for 1-3 hours.

[0064] Embodiment 3

[0065] The two-component PUR (moisture curing hot melt adhesive) preparation process includes the following steps:

[0066] Preparation of Component A

[0067] Raw material preparation: Polytetramethylene glycol (PTMG) with a molecular weight of 3000-4000: 150 g;

[0068] Toluene diisocyanate (TDI): 300 g;

[0069] Oxalic acid: 0.75 g;

[0070] Liquid paraffin: 15 g.

[0071] Preparation steps: 150 g of polytetrahydrofuran diol (PTMG) and 300 g of toluene diisocyanate (TDI) are added into a reaction kettle, heated to 120° C., stirred and reacted for 3 hours under nitrogen protection to obtain a prepolymer;

[0072] After the reaction was completed, 0.75 g of oxalic acid was added to the reactor as an inhibitor and stirring was continued for 10 minutes;

[0073] Then add 15 g of liquid paraffin as a surface sealant, and continue stirring for 10 minutes until the mixture is evenly mixed to obtain component A.

[0074] Preparation of component B

[0075] Raw material preparation: polyethylene terephthalate (PET) with a molecular weight of 2000-3000: 150 g;

[0076] Ethylenediamine (EDA) with a molecular weight of 4000-5000: 150 g;

[0077] Methylene diphenyl diisocyanate (MDI): 75 g.

[0078] Preparation steps: 150 g of polyethylene terephthalate (PET) and 150 g of ethylenediamine (EDA) were added to a reaction kettle, heated to 180° C., stirred and mixed evenly under nitrogen protection, and then slowly cooled to 60° C.;

[0079] After cooling to 60°C, add 75 g of diphenylmethane diisocyanate (MDI), control the R value to 0.5, and continue stirring for 30 minutes until the mixture is evenly mixed to obtain component B.

[0080] How to use

[0081] Preheating: Preheat component A to 100°C and component B to 80°C to ensure that both components have good fluidity;

[0082] Mixing: Mix the preheated component A and component B in a weight ratio of 1:1.5 using a two-component glue gun, and control the R value to 1.5;

[0083] Construction: Apply the mixed glue evenly on the surface of the material to be bonded and cure it at room temperature for 1-3 hours.

[0084] Embodiment 4

[0085] The two-component PUR (moisture curing hot melt adhesive) preparation process includes the following steps:

[0086] Preparation of Component A

[0087] Raw material preparation: polyethylene glycol (PEG) with a molecular weight of 1500-2500: 130 g;

[0088] Methylene diphenyl diisocyanate (MDI): 260 g;

[0089] Benzoic acid: 0.65 g;

[0090] Liquid paraffin: 13 grams.

[0091] Preparation steps: 130 g of polyethylene glycol (PEG) and 260 g of diphenylmethane diisocyanate (MDI) were added to a reaction kettle, heated to 100° C., stirred and reacted for 3 hours under nitrogen protection to obtain a prepolymer;

[0092] After the reaction was completed, 0.65 g of benzoic acid was added to the reactor as a polymerization inhibitor and stirring was continued for 10 minutes;

[0093] Then add 13 g of liquid paraffin as a surface sealant, and continue stirring for 10 minutes until the mixture is uniformly mixed to obtain component A.

[0094] Preparation of component B

[0095] Raw material preparation: polyethylene adipate (PBA) with a molecular weight of 1000-2000: 130 g;

[0096] Diethylenetriamine (DETA) with a molecular weight of 2000-3000: 130 g;

[0097] Methylene diphenyl diisocyanate (MDI): 65 g.

[0098] Preparation steps: 130 g of polyethylene adipate (PBA) and 130 g of diethylenetriamine (DETA) were added to a reaction kettle, heated to 180° C., stirred and mixed evenly under nitrogen protection, and then slowly cooled to 60° C.;

[0099] After cooling to 60°C, 65 g of diphenylmethane diisocyanate (MDI) was added, the R value was controlled to be 0.5, and stirring was continued for 30 minutes until the mixture was uniformly mixed to obtain component B.

[0100] How to use

[0101] Preheating: Preheat component A to 85°C and component B to 65°C to ensure that the two components have good fluidity;

[0102] Mixing: Mix the preheated component A and component B in a weight ratio of 1:1.1 using a two-component glue gun, and control the R value to 1.35;

[0103] Construction: Apply the mixed glue evenly on the surface of the material to be bonded and cure it at room temperature for 1-3 hours.

[0104] Embodiment 5

[0105] The two-component PUR (moisture curing hot melt adhesive) preparation process includes the following steps:

[0106] Preparation of Component A

[0107] Raw material preparation: Polypropylene glycol (PPG) with a molecular weight of 2000-3000: 140 g;

[0108] Isophorone diisocyanate (IPDI): 280 g;

[0109] Acetic acid: 0.7 g;

[0110] Liquid paraffin: 14 g.

[0111] Preparation steps: 140 g of polypropylene glycol (PPG) and 280 g of isophorone diisocyanate (IPDI) were added into a reaction kettle, heated to 110° C., stirred and reacted for 3 hours under nitrogen protection to obtain a prepolymer;

[0112] After the reaction was completed, 0.7 g of acetic acid was added to the reactor as an inhibitor and stirring was continued for 10 minutes;

[0113] Then add 14 g of liquid paraffin as a surface sealant, and continue stirring for 10 minutes until the mixture is uniformly mixed to obtain component A.

[0114] Preparation of component B

[0115] Raw material preparation: Polybutylene adipate (PBD) with a molecular weight of 1500-2500: 140 g;

[0116] Triethylenetetramine (TETA) with a molecular weight of 3000-4000: 140 g;

[0117] Methylene diphenyl diisocyanate (MDI): 70 g.

[0118] Preparation steps: 140 g of polybutylene adipate (PBD) and 140 g of triethylenetetramine (TETA) were added to a reaction kettle, heated to 180° C., stirred and mixed evenly under nitrogen protection, and then slowly cooled to 60° C.;

[0119] After cooling to 60°C, add 70 g of diphenylmethane diisocyanate (MDI), control the R value to 0.5, and continue stirring for 30 minutes until the mixture is evenly mixed to obtain component B.

[0120] How to use

[0121] Preheating: Preheat component A to 95°C and component B to 75°C to ensure that the two components have good fluidity;

[0122] Mixing: Mix the preheated component A and component B thoroughly in a weight ratio of 1:1.3 using a two-component glue gun, and control the R value to 1.45;

[0123] Construction: Apply the mixed glue evenly on the surface of the material to be bonded and cure it at room temperature for 1-3 hours.

[0124] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations may be made to the embodiments without departing from the principles and spirit thereof, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. Two-component PUR (moisture curing hot melt adhesive), including component A and component B, wherein: Component A is a prepolymer prepared by reacting a diol with a molecular weight of 1000-5000 with a diisocyanate, an organic acid is added as an inhibitor, and appropriate liquid paraffin is added as a surface sealant; Component B is prepared by melting and mixing polyester polyol with good crystallinity of molecular weight 1000-3000 and dibasic polyetheramine with molecular weight 2000-5000 at high temperature, cooling to below 60°C, adding measured diisocyanate, controlling R value between 0.3-0.7, and obtaining hydroxyl terminated resin part.

2. The two-component PUR (moisture curing hot melt adhesive) according to claim 1, characterized in that: The diol is selected from one or more of polyethylene glycol, polypropylene glycol and polytetrahydrofuran diol.

3. The two-component PUR (moisture curing hot melt adhesive) according to claim 1, characterized in that: The diisocyanate is selected from one or more of toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), and isophorone diisocyanate (IPDI).

4. The two-component PUR (moisture curing hot melt adhesive) according to claim 1, characterized in that: The organic acid is selected from one or more of benzoic acid, acetic acid and oxalic acid.

5. The two-component PUR (moisture curing hot melt adhesive) according to claim 1, characterized in that: The polyester polyol is selected from one or more of polyethylene adipate, polybutylene adipate and polyethylene terephthalate.

6. The two-component PUR (moisture curing hot melt adhesive) according to claim 1, characterized in that: The divalent polyetheramine is selected from one or more of ethylenediamine, diethylenetriamine and triethylenetetramine.

7. The preparation process of two-component PUR (moisture curing hot melt adhesive) according to claim 1, characterized in that: The following steps are involved: Preparation of component A: react diol with a molecular weight of 1000-5000 with diisocyanate at a certain temperature to prepare a prepolymer, then add an organic acid as an inhibitor, and then add an appropriate amount of liquid paraffin as a surface sealant, and mix well; Preparation of component B: melt and mix polyester polyol with good crystallinity and molecular weight of 1000-3000 and dibasic polyetheramine with molecular weight of 2000-5000 at high temperature, cool to below 60°C, add measured diisocyanate, control R value between 0.3-0.7, and obtain hydroxyl-terminated resin part; When in use, preheat component A and component B to a good fluidity state respectively, mix them thoroughly with a two-component glue gun, control the R value between 1.2-1.5, and prepare the moisture-curing hot melt adhesive PUR.

8. The process for preparing a two-component PUR (moisture curing hot melt adhesive) according to claim 7, characterized in that: During the preparation of component A, the reaction temperature is 80-120° C. and the reaction time is 2-4 hours.

9. The process for preparing a two-component PUR (moisture curing hot melt adhesive) according to claim 7, characterized in that: During the preparation of the B component, the high temperature melting temperature is 150-200° C., and the cooling rate after uniform mixing is 1-2° C. / min.