CN108659771A - A kind of preparation method of water-proof environmental protection polyurethane adhesive - Google Patents
A kind of preparation method of water-proof environmental protection polyurethane adhesive Download PDFInfo
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- CN108659771A CN108659771A CN201810389675.8A CN201810389675A CN108659771A CN 108659771 A CN108659771 A CN 108659771A CN 201810389675 A CN201810389675 A CN 201810389675A CN 108659771 A CN108659771 A CN 108659771A
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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
- C09J175/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation methods of water-proof environmental protection polyurethane adhesive, include the following steps：Xanthans is added in carbodiimides aqueous solution and is stirred, regulation system pH value is 6.2 6.6, and glutamic acid is added and continues to stir to get first material；Benzene dimethylene diisocyanate, polycaprolactone diols, first material, polysiloxane is soluble in water, heating, it is persistently stirred in temperature-rise period, it is subsequently added into disproportionated rosin, tertiarybutyldiethanolamine continues to stir, it is 7.5 8.4 to adjust reaction solution pH, continue to stir, cooling obtains second material；Into second material, addition trimethylolethane, dipropylene glycol, aqueous alkide resin, which are uniformly mixed, obtains water-proof environmental protection polyurethane adhesive.Gained adhesive bonds intensity of the invention is high, and fire-retardant, high temperature resistant, water resistance is excellent, and environmentally protective, is free of organic solvent, overcomes pollution of the organic solvent to environment.
Description
Technical field
The present invention relates to technical field of polyurethane adhesive more particularly to a kind of preparations of water-proof environmental protection polyurethane adhesive
Method.
Background technology
In building materials field, most of producers are still continuing to use two part solvent type adhesive.Two part solvent type gluing
Agent, lower machine need to cure, and energy consumption is very high, in use a large amount of solvent direct emissions, and not only environmental pollution is big, but also country wants
Corresponding bond strength and stability should be had as building materials use by asking.
Invention content
Technical problems based on background technology, the present invention propose a kind of preparation of water-proof environmental protection polyurethane adhesive
Method, gained adhesive bonds intensity is high, and stability is excellent, and environmentally protective, is free of organic solvent, overcomes organic molten
Pollution of the agent to environment.
A kind of preparation method of water-proof environmental protection polyurethane adhesive proposed by the present invention, includes the following steps：
S1, xanthans is added in carbodiimides aqueous solution and is stirred, regulation system pH value is 6.2-6.6, and paddy ammonia is added
Acid continues to stir to get first material；
S2, benzene dimethylene diisocyanate, polycaprolactone diols, first material, polysiloxane are dissolved in water
In, it heats up, is persistently stirred in temperature-rise period, be subsequently added into disproportionated rosin, tertiarybutyldiethanolamine continues to stir, adjusting reaction solution
PH is 7.5-8.4, continues to stir, and cooling obtains second material；
S3, into second material, addition trimethylolethane, dipropylene glycol, aqueous alkide resin are uniformly mixed and obtain
Water-proof environmental protection polyurethane adhesive.
Preferably, in S1, carbodiimides concentration of aqueous solution is 0.4-0.8wt%, and xanthans, carbodiimides are water-soluble
Liquid, glutamic acid weight ratio be 30-50：80-120：10-20.
Preferably, in S1, xanthans is added in carbodiimides aqueous solution and stirs 4-8h, mixing speed 300-
500r/min, whipping temp are 60-80 DEG C, use hydrochloric acid regulation system pH value for 6.2-6.6, and glutamic acid is added and continues to stir
40-80min, whipping temp are 75-85 DEG C, and mixing speed 1000-1500r/min obtains first material.
Preferably, in S2, benzene dimethylene diisocyanate, polycaprolactone diols, first material, poly organo
Alkane, water, disproportionated rosin, tertiarybutyldiethanolamine weight ratio be 60-80：10-20：6-12：14-20：80-120：1-2：1-2.
Preferably, in S2, by benzene dimethylene diisocyanate, polycaprolactone diols, first material, poly organo
Alkane is soluble in water, from room temperature to 90-100 DEG C, is persistently stirred in temperature-rise period, is subsequently added into disproportionated rosin, tertiary butyl two
Ethanol amine continues to stir, and it is 7.5-8.4 to adjust reaction solution pH with sodium hydroxide, continues to stir 20-40min, be cooled to room temperature
To second material.
Preferably, in S3, second material, trimethylolethane, dipropylene glycol, aqueous alkide resin weight ratio be
120-140：1-2：1-2：1-2.
Gained adhesive bonds intensity of the invention is high, and fire-retardant, high temperature resistant, water resistance is excellent, and environmentally protective, is free of
Organic solvent overcomes pollution of the organic solvent to environment.
In S1 of the present invention, due to having a large amount of hydroxyl, carboxyl and amino in xanthan gum structure, there is extremely strong hydrophily,
Xanthans is crosslinked in carbodiimides solution with the amino of glutamic acid and carboxyl, stickiness increase it is apparent, and have compared with
Low water imbibition, and the polyglutamic acid that end is formed and the dispersion of benzene dimethylene diisocyanate, polycaprolactone diols are imitated
Fruit is good, can effectively improve the initial adhesion force of polyurethane adhesive, then after carrying out epoxy cross-linking with aqueous alkide resin, water resistance and power
It learns performance and has obtained further raising；And use benzene dimethylene diisocyanate, polycaprolactone diols and first material,
Polysiloxane mixes crosslinking according to a certain ratio, and improving can the high temperature resistant of polyurethane adhesive, water-fast and weather resistance.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of water-proof environmental protection polyurethane adhesive, includes the following steps：
S1,30kg xanthans is added in a concentration of 0.4wt% carbodiimides aqueous solutions of 120kg and stirs 8h, stirring speed
Degree is 300r/min, and whipping temp is 80 DEG C, uses hydrochloric acid regulation system pH value for 6.2-6.6, and 10kg glutamic acid is added and continues
80min is stirred, whipping temp is 75 DEG C, and mixing speed 1500r/min obtains first material；
S2, by 60kg benzene dimethylene diisocyanate, 20kg polycaprolactone diolss, 6kg first materials, 20kg is poly- has
Organic siloxane is dissolved in 80kg water, from room temperature to 100 DEG C, is persistently stirred in temperature-rise period, and 1kg disproportionation pines are subsequently added into
Fragrant, 2kg tertiarybutyldiethanolamines continue to stir, and it is 7.5-8.4 to adjust reaction solution pH with sodium hydroxide, continue to stir 20min, cold
But second material is obtained to room temperature；
S3,1kg trimethylolethanes, 2kg dipropylene glycols, 1kg water alcohol acid trees are added into 140kg second materials
Fat is uniformly mixed and obtains water-proof environmental protection polyurethane adhesive.
Embodiment 2
A kind of preparation method of water-proof environmental protection polyurethane adhesive, includes the following steps：
S1,50kg xanthans is added in a concentration of 0.8wt% carbodiimides aqueous solutions of 80kg and stirs 4h, mixing speed
For 500r/min, whipping temp is 60 DEG C, uses hydrochloric acid regulation system pH value for 6.2-6.6, and 20kg glutamic acid is added and continues to stir
40min is mixed, whipping temp is 85 DEG C, and mixing speed 1000r/min obtains first material；
S2,80kg benzene dimethylene diisocyanate, 10kg polycaprolactone diolss, 12kg first materials, 14kg are gathered
Organosiloxane is dissolved in 120kg water, from room temperature to 90 DEG C, is persistently stirred in temperature-rise period, and 2kg disproportionation pines are subsequently added into
Fragrant, 1kg tertiarybutyldiethanolamines continue to stir, and it is 7.5-8.4 to adjust reaction solution pH with sodium hydroxide, continue to stir 40min, cold
But second material is obtained to room temperature；
S3,2kg trimethylolethanes, 1kg dipropylene glycols, 2kg water alcohol acid trees are added into 120kg second materials
Fat is uniformly mixed and obtains water-proof environmental protection polyurethane adhesive.
Embodiment 3
A kind of preparation method of water-proof environmental protection polyurethane adhesive, includes the following steps：
S1,35kg xanthans is added in a concentration of 0.5wt% carbodiimides aqueous solutions of 110kg and stirs 7h, stirring speed
Degree is 350r/min, and whipping temp is 75 DEG C, uses hydrochloric acid regulation system pH value for 6.2-6.6, and 12kg glutamic acid is added and continues
70min is stirred, whipping temp is 78 DEG C, and mixing speed 1400r/min obtains first material；
S2, by 65kg benzene dimethylene diisocyanate, 18kg polycaprolactone diolss, 8kg first materials, 18kg is poly- has
Organic siloxane is dissolved in 90kg water, from room temperature to 96 DEG C, is persistently stirred in temperature-rise period, and 1.2kg disproportionation pines are subsequently added into
Fragrant, 1.7kg tertiarybutyldiethanolamines continue to stir, and it is 7.5-8.4 to adjust reaction solution pH with sodium hydroxide, continue to stir 25min,
It is cooled to room temperature to obtain second material；
S3, into 135kg second materials, addition 1.2kg trimethylolethanes, 1.7kg dipropylene glycols, 1.4kg are aqueous
Alkyd resin is uniformly mixed and obtains water-proof environmental protection polyurethane adhesive.
Embodiment 4
A kind of preparation method of water-proof environmental protection polyurethane adhesive, includes the following steps：
S1,45kg xanthans is added in a concentration of 0.7wt% carbodiimides aqueous solutions of 90kg and stirs 5h, mixing speed
For 450r/min, whipping temp is 65 DEG C, uses hydrochloric acid regulation system pH value for 6.2-6.6, and 18kg glutamic acid is added and continues to stir
50min is mixed, whipping temp is 82 DEG C, and mixing speed 1200r/min obtains first material；
S2,75kg benzene dimethylene diisocyanate, 12kg polycaprolactone diolss, 10kg first materials, 16kg are gathered
Organosiloxane is dissolved in 110kg water, from room temperature to 94 DEG C, is persistently stirred in temperature-rise period, and 1.8kg disproportionations are subsequently added into
Rosin, 1.3kg tertiarybutyldiethanolamines continue to stir, and it is 7.5-8.4 to adjust reaction solution pH with sodium hydroxide, continues to stir
35min is cooled to room temperature to obtain second material；
S3, into 125kg second materials, addition 1.8kg trimethylolethanes, 1.3kg dipropylene glycols, 1.6kg are aqueous
Alkyd resin is uniformly mixed and obtains water-proof environmental protection polyurethane adhesive.
Embodiment 5
A kind of preparation method of water-proof environmental protection polyurethane adhesive, includes the following steps：
S1,40kg xanthans is added in a concentration of 0.6wt% carbodiimides aqueous solutions of 100kg and stirs 6h, stirring speed
Degree is 400r/min, and whipping temp is 70 DEG C, uses hydrochloric acid regulation system pH value for 6.2-6.6, and 15kg glutamic acid is added and continues
60min is stirred, whipping temp is 80 DEG C, and mixing speed 1300r/min obtains first material；
S2, by 70kg benzene dimethylene diisocyanate, 15kg polycaprolactone diolss, 9kg first materials, 17kg is poly- has
Organic siloxane is dissolved in 100kg water, from room temperature to 95 DEG C, is persistently stirred in temperature-rise period, and 1.5kg disproportionation pines are subsequently added into
Fragrant, 1.5kg tertiarybutyldiethanolamines continue to stir, and it is 7.5-8.4 to adjust reaction solution pH with sodium hydroxide, continue to stir 30min,
It is cooled to room temperature to obtain second material；
S3, into 130kg second materials, addition 1.5kg trimethylolethanes, 1.5kg dipropylene glycols, 1.5kg are aqueous
Alkyd resin is uniformly mixed and obtains water-proof environmental protection polyurethane adhesive.
5 gained water-proof environmental protection polyurethane adhesive of embodiment and commercially available environmental-protection polyurethane adhesive are tested for the property；
Emulsion appearance and stability：Sample is stored at room temperature some time, is observed at interval of 7d, and to precipitate
Time as measurement index；
Viscosity test：Using BrookfieldDV-IIPro+ type rotational viscometers, at a temperature of 25 DEG C, according to GB/T
2794-1995 standards carry out viscosimetric analysis to each samples of latex；
Peel strength test：Polyethylene (PE)/polypropylene (PP) film water-based polyurethane adhesive is compound, 50 DEG C of bakings
Cure for 24 hours in case；Laminated film is cut into the sample of 200mm × 25mm, by GB/T2791-1995 CMT7000 type electronics
Universal testing machine is tested (rate of extension 100mm/min) to the T-type peel strength of sample, is repeated 5 times, is averaged；
Hardening time：Isometric each sample is coated on glass dish, coating thickness 5mm sees drying the time.
Its result is as follows：
| Embodiment 5 | Commercially available environmental-protection polyurethane adhesive | |
| Stability | Stablize | Stablize |
| Viscosity, cp | 58 | 40 |
| Peel strength, N/cm | 3.3 | 1.2 |
| Hardening time, min | 1 | 8 |
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of water-proof environmental protection polyurethane adhesive, which is characterized in that include the following steps：
S1, will xanthans be added carbodiimides aqueous solution in stir, regulation system pH value be 6.2-6.6, be added glutamic acid after
It is continuous to stir to get first material；
S2, benzene dimethylene diisocyanate, polycaprolactone diols, first material, polysiloxane is soluble in water, liter
Temperature persistently stirs in temperature-rise period, is subsequently added into disproportionated rosin, tertiarybutyldiethanolamine continues to stir, and adjusts reaction solution pH and is
7.5-8.4 continues to stir, and cooling obtains second material；
S3, into second material, addition trimethylolethane, dipropylene glycol, aqueous alkide resin are uniformly mixed and obtain waterproof
Environmental-protection polyurethane adhesive.
2. the preparation method of water-proof environmental protection polyurethane adhesive according to claim 1, which is characterized in that in S1, carbonization two
Imines concentration of aqueous solution be 0.4-0.8wt%, xanthans, carbodiimides aqueous solution, glutamic acid weight ratio be 30-50：80-
120：10-20.
3. the preparation method of water-proof environmental protection polyurethane adhesive according to claim 1 or claim 2, which is characterized in that, will be yellow in S1
Virgin rubber, which is added in carbodiimides aqueous solution, stirs 4-8h, and mixing speed 300-500r/min, whipping temp is 60-80 DEG C,
It uses hydrochloric acid regulation system pH value for 6.2-6.6, glutamic acid is added and continues to stir 40-80min, whipping temp is 75-85 DEG C, is stirred
It is 1000-1500r/min to mix speed, obtains first material.
4. according to the preparation method of any one of the claim 1-3 water-proof environmental protection polyurethane adhesives, which is characterized in that S2
In, benzene dimethylene diisocyanate, polycaprolactone diols, first material, polysiloxane, water, disproportionated rosin, tertiary fourth
The weight ratio of base diethanol amine is 60-80：10-20：6-12：14-20：80-120：1-2：1-2.
5. according to the preparation method of any one of the claim 1-4 water-proof environmental protection polyurethane adhesives, which is characterized in that S2
In, benzene dimethylene diisocyanate, polycaprolactone diols, first material, polysiloxane is soluble in water, from room temperature
It is warming up to 90-100 DEG C, is persistently stirred in temperature-rise period, is subsequently added into disproportionated rosin, tertiarybutyldiethanolamine continues to stir, use
It is 7.5-8.4 that sodium hydroxide, which adjusts reaction solution pH, continues to stir 20-40min, is cooled to room temperature to obtain second material.
6. according to the preparation method of any one of the claim 1-5 water-proof environmental protection polyurethane adhesives, which is characterized in that S3
In, second material, trimethylolethane, dipropylene glycol, aqueous alkide resin weight ratio be 120-140：1-2：1-2：
1-2。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810389675.8A CN108659771A (en) | 2018-04-27 | 2018-04-27 | A kind of preparation method of water-proof environmental protection polyurethane adhesive |
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| CN201810389675.8A CN108659771A (en) | 2018-04-27 | 2018-04-27 | A kind of preparation method of water-proof environmental protection polyurethane adhesive |
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| CN108659771A true CN108659771A (en) | 2018-10-16 |
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| CN201810389675.8A Withdrawn CN108659771A (en) | 2018-04-27 | 2018-04-27 | A kind of preparation method of water-proof environmental protection polyurethane adhesive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234761A (en) * | 2020-03-17 | 2020-06-05 | 北京华腾新材料股份有限公司 | Single-component solvent-free polyurethane adhesive and preparation method thereof |
-
2018
- 2018-04-27 CN CN201810389675.8A patent/CN108659771A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234761A (en) * | 2020-03-17 | 2020-06-05 | 北京华腾新材料股份有限公司 | Single-component solvent-free polyurethane adhesive and preparation method thereof |
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Application publication date: 20181016 |