CN101402840B

CN101402840B - Process for producing frost resistant polyurethane viscose glue

Info

Publication number: CN101402840B
Application number: CN200810201412A
Authority: CN
Inventors: 程诗强; 陈县萍
Original assignee: SHANGHAI JIUYUAN PETROCHEMICAL CO Ltd
Current assignee: SHANGHAI JIUYUAN PETROCHEMICAL CO Ltd
Priority date: 2008-10-20
Filing date: 2008-10-20
Publication date: 2012-09-05
Anticipated expiration: 2028-10-20
Also published as: CN101402840A

Abstract

The invention relates to the technical field of a polymer material and chemical industry, in particular to a preparation method of frost resistance polyurethane glue, which is characterized in that: isocyanate or an isocyanate compound B, polyester polyol C with symmetrical structure, and a catalyst D are added into an organic solvent A for reaction for 2 to 5 hours at 50 and 100 DEG C; then a chain extendor E is added for reaction for 1 to 4 hours; the temperature is reduced to 35 to 60 DEG C; an organic solvent F of 10 to 25 percent is added for dilution to achieve solid content of 35 to 65percent; a frost resistance modifier G is added for stirring; then 0 to 10 percent of other accessory ingredients are added for fully stirring; the temperature is reduced to be 20 to 35 DEG C; and then the mixture is filtered and packaged for obtaining the finished product. The adding amount of the frost resistance modifier G accounts for 0.01 to 10 percent of the weight of the finished frost resistance polyurethane glue system. Compared with the prior art, the preparation method of the frost resistance polyurethane glue can be used under a condition of minus15 DEG C to 5 DEG C, thus reducingthe storage and use temperature of the glue, and therefore can be broadly applied to the industries of vehicles and furniture.

Description

A kind of preparation method of frost resistance polyurethane glue

[technical field]

The present invention relates to macromolecular material and chemical technology field, is a kind of preparation method of frost resistance polyurethane glue specifically.

[background technology]

Polyurethane adhesive with highly crystalline performance has fast doing and the good advantage of cohesive strength; But because the frozen glue problem, temperature severe cold zone particularly in the winter time has a strong impact on and uses and deposit; In the conventional use; Manufacturing enterprise and user have to build that insulated building is deposited or before using, adopt various heating measures, and recovering the use properties of glue, this just makes and stores and use numerous and diverse while that becomes increases cost greatly.

[summary of the invention]

The objective of the invention is to make polyurethane glue under-10 ℃ of conditions, to deposit and to use with highly crystalline structure.

For realizing above-mentioned purpose; Design a kind of preparation method of frost resistance polyurethane glue; It is characterized in that forming: in 20～25% middle high boiling organic solvent A, add 18～30% isocyanic ester or isocyanate mixture B, 20～35% polyester polyol C, 0.01～0.1% catalyzer D, under 50～100 ℃, reacted 2～5 hours then, add 0.5～2% chainextender E again and further reacted 1-4 hour with symplex structure by following weight percent feedstock production; Be cooled to 35-60 ℃ then; Adding 10～25% organic solvent F again, to be diluted to solid content be 35～65%, adds freeze proof properties-correcting agent G and stir 30～90min with the speed of 800～1200 commentaries on classics/min, adds 0～10% other auxiliary agents more as required; Fully mix 30～90min; Be cooled to 20～35 ℃ then, filter and package and get product, the add-on of said freeze proof properties-correcting agent G accounts for 0.01%～10% of finished product frost resistant polyurethane viscose glue system weight per-cent; The mixture of one or more in the described freeze proof properties-correcting agent G employing diesel pour inhibitor; High boiling organic solvent A is that boiling point is at the non-aromatic hydrocarbons organic solvent more than 90 ℃ in described; Described organic solvent F is one or more in acetone, butanone, pimelinketone, the vinyl acetic monomer.

Described boiling point is at least a in N-BUTYL ACETATE, the N ' dinethylformamide at the non-aromatic hydrocarbons organic solvent more than 90 ℃.

Described isocyanic ester or isocyanate mixture B are meant one or more mixtures in diphenylmethanediisocyanate, the tolylene diisocyanate.

Described polyester polyol C with symplex structure for through after the 100-130 ℃ of vacuum hydro-extraction contain two hydroxyls and carbonatoms is the polyester polyol of even numbers.

Described catalyzer D is one or more the mixture that has in dibutyl tin dilaurate, stannous octoate, dibutyltin diacetate, triethylenediamine, quadrol, the tn.

Described chainextender E is one or more the mixture in divalent alcohol or the diamine.

Described other auxiliary agent is one or more the mixture in inhibitor, uv-absorbing agent, the photostabilizer, and this auxiliary agent not necessarily can add as required.

The present invention compared with prior art, the product of preparation can use under-15 ℃～5 ℃ conditions, has reduced glue storage and use temperature, can be widely used in automobile and furniture industry.

[embodiment]

Be further described in the face of the present invention down.

The trade mark of related products among the following embodiment is the product of Shanghai Jiuyuan Petroleum Chemical Co., Ltd., like freeze proof properties-correcting agent G, can adopt among the present commercially available trade mark diesel pour inhibitor JY8500/JY9508/JY9053 any; Inhibitor can adopt 1010/BHT/1098/1135/JY-Stab 8733 in other auxiliary agent, and uv-absorbing agent can adopt UV-328/UV-P/UV-320, and photostabilizer can adopt 770/944/B75 etc.

Embodiment 1:

At first add the mixed organic solvents A that N-BUTYL ACETATE 80g and N ' N-dimethylformamide 80g form, thorough mixing progressively adds B with the rotating speed of 600～1000 commentaries on classics/min: tolylene diisocyanate 200g while stirring; C: polyethylene glycol adipate 100g and poly adipate succinic acid ester 100g, D: dibutyl tin dilaurate 0.2g is warming up to 50～100 ℃ and reacts 2～5h; Add E:1 again, 4-butyleneglycol 5g reacts 2.5h, is cooled to 35-60 ℃ then; Add the mixed organic solvents F that butanone 54g and vinyl acetic monomer 54g form, the trade mark that adds 11g again is the freeze proof properties-correcting agent G of JY8500, fully mixes 1h; The trade mark that adds 8g at last is that the oxidation inhibitor of JY-Stab 8733 is as auxiliary agent; Fully mix 45min, system reduced to room temperature, filter and package finished product.

Embodiment 2:

At first adding A:N ' N-dimethylformamide 150g, is that 600～1000 commentaries on classics/min progressively add B while stirring with rotating speed: the diphenylmethanediisocyanate 100g of modification and tolylene diisocyanate 50g, C: poly adipate succinic acid ester 190g; D: dibutyl tin dilaurate 0.1g is warming up to 50～100 ℃ and reacts 2～5h, adds E again: TriMethylolPropane(TMP) 4g reacts 2.5h; Be cooled to 35～60 ℃ then; Add F: butanone 100g, adding the 5g trade mark again is the freeze proof properties-correcting agent G of JY9508, fully mixes 1h; System is reduced to room temperature, filter and package finished product.

Embodiment 3:

At first add A: N-BUTYL ACETATE 180g is that 600～1000 commentaries on classics/min progressively add B while stirring with rotating speed: the diphenylmethanediisocyanate 160g of modification, C: polyethylene glycol adipate 150g and poly adipate succinic acid ester 50g; D: dibutyl tin dilaurate 0.1g is warming up to 50～100 ℃ and reacts 2～5h, adds E:1 again; 4-butyleneglycol 9g reacts 2h, is cooled to 35～60 ℃ then, adds F: vinyl acetic monomer 100g; Adding the 15g trade mark again is the freeze proof properties-correcting agent G of JY9053; Fully mix 1h, the uv-absorbing agent that adds the 8g trade mark at last and be UV-328 is as auxiliary agent, thorough mixing 30min; System is reduced to room temperature, filter and package finished product.

Claims

1. preparation method of frost resistance polyurethane glue; It is characterized in that forming: the isocyanic ester of adding 18～30% or isocyanate mixture (B), 20～35% the polyester polyol with symplex structure (C), 0.01～0.1% catalyzer (D) in 20～25% middle high boiling organic solvent (A) by following weight percent feedstock production; Under 50～100 ℃, reacted 2～5 hours then; Add 0.5～2% chainextender (E) again and further reacted 1-4 hour, be cooled to 35-60 ℃ then, adding 10～25% organic solvents (F) again, to be diluted to solid content be 35～65%; Add the speed stirring 30～90min of freeze proof properties-correcting agent (G) with 800～1200 commentaries on classics/min; Add 0～10% other auxiliary agents more as required, fully mix 30～90min, be cooled to 20～35 ℃ then; Filter and package and get product, the add-on of said freeze proof properties-correcting agent (G) accounts for 0.01%～10% of finished product frost resistant polyurethane viscose glue system weight per-cent; The mixture of one or more in described freeze proof properties-correcting agent (G) the employing diesel pour inhibitor; High boiling organic solvent (A) is that boiling point is at the non-aromatic hydrocarbons organic solvent more than 90 ℃ in described; Described organic solvent (F) is one or more in acetone, butanone, pimelinketone, the vinyl acetic monomer.

2. a kind of preparation method of frost resistance polyurethane glue as claimed in claim 1 is characterized in that: described boiling point is at least a in N-BUTYL ACETATE, the N ' dinethylformamide at the non-aromatic hydrocarbons organic solvent more than 90 ℃.

3. a kind of preparation method of frost resistance polyurethane glue as claimed in claim 1 is characterized in that: described isocyanic ester or isocyanate mixture (B) are meant one or more mixtures in diphenylmethanediisocyanate, the tolylene diisocyanate.

4. a kind of preparation method of frost resistance polyurethane glue as claimed in claim 1 is characterized in that: described polyester polyol (C) with symplex structure for through after the 100-130 ℃ of vacuum hydro-extraction contain two hydroxyls and carbonatoms is the polyester polyol of even numbers.

5. a kind of preparation method of frost resistance polyurethane glue as claimed in claim 1 is characterized in that: described catalyzer (D) is for there being one or more the mixture in dibutyl tin dilaurate, stannous octoate, dibutyltin diacetate, triethylenediamine, quadrol, the tn.

6. a kind of preparation method of frost resistance polyurethane glue as claimed in claim 1 is characterized in that: described chainextender (E) is one or more the mixture in divalent alcohol or the diamine.

7. a kind of preparation method of frost resistance polyurethane glue as claimed in claim 1 is characterized in that: described other auxiliary agent is one or more the mixture in the inhibitor that dissolves in acetone, butanone solvent, uv-absorbing agent, the photostabilizer.