CN106189997A - Use timber floor and the heat treatment method thereof of organic silicon modified polyurethane adhesive - Google Patents
Use timber floor and the heat treatment method thereof of organic silicon modified polyurethane adhesive Download PDFInfo
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- CN106189997A CN106189997A CN201610584800.1A CN201610584800A CN106189997A CN 106189997 A CN106189997 A CN 106189997A CN 201610584800 A CN201610584800 A CN 201610584800A CN 106189997 A CN106189997 A CN 106189997A
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
-
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- 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
- C08G18/61—Polysiloxanes
-
- 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
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic 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
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/02—Flooring or floor layers composed of a number of similar elements
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Architecture (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention discloses a kind of timber floor using organic silicon modified polyurethane adhesive and heat treatment method thereof.The present invention includes substrate, and the upper strata of substrate is pasted with epidermis through adhesive, is pasted with base plate through adhesive below substrate, and substrate is the finger-jointed plate pasted through adhesive by wooden unit；Described adhesive is made up of following raw materials according by weight: polyisocyanates 5 20 parts, containing active hydrogen silicone oil 1 20 parts, polyhydric alcohol 30 50 parts, plasticizer 10 30 parts, catalyst 0.05 0.20 parts, defoamer 0.5 3 parts, deicer 0.02 0.20 parts, coupling agent 0.02 0.30 parts, antioxidant 0.02 0.15 parts.The present invention is possible not only to be greatly improved mechanical property, and has superior thermostability, resistance to water.
Description
Technical field
The present invention relates to a kind of timber floor using organic silicon modified polyurethane adhesive and heat treatment method thereof, belong to wood
Floor, particularly relate to the production technical field on grafting floor.
Background technology
Along with rapid economic development, stepping up of living standards of the people, the consumption of timber increases further, causes me
The rise of state's wooden product price, solid wooden floor board and the multi-layer solid wood floor price with rare tree as veneer climb up and up.In order to
Alleviate the imbalance between supply and demand of Solid Wood Flooring Markets, also for the rare tree of protection China, it is achieved sustainable development, how by renewable
Material such as plastic applications, in making in timber floor, becomes the task of top priority of the most numerous timber floor producer.Also have now
Manufacturer produces the finger joint wood floor being spliced by waste wood, but owing to this kind of floor strength is the most up to standard, therefore makes
With the most extensive.And the biggest reason limiting finger joint wood floor mechanical property to be the adherence force of adhesive not ideal enough,
The most how to improve existing adhesive, thus research and develop that a splicing intensity is high, extreme environment adaptability is good, length in service life
Timber floor, becomes a difficult problem urgently to be resolved hurrily.
Summary of the invention
It is an object of the invention to, it is provided that a kind of timber floor using organic silicon modified polyurethane adhesive and heat treatment thereof
Method.The present invention is possible not only to be greatly improved mechanical property, and has superior thermostability, resistance to water.
Technical scheme: a kind of timber floor using organic silicon modified polyurethane adhesive, including substrate, substrate
Upper strata be pasted with epidermis through adhesive, be pasted with base plate through adhesive below substrate, substrate be by wooden unit through adhesive paste
Finger-jointed plate；Described adhesive is made up of following raw materials according by weight:
Polyisocyanates 5-20 part,
Containing active hydrogen silicone oil 1-20 part,
Polyhydric alcohol 30-50 part,
Plasticizer 10-30 part,
Catalyst 0.05-0.20 part,
Defoamer 0.5-3 part,
Deicer 0.02-0.20 part,
Coupling agent 0.02-0.30 part,
Antioxidant 0.02-0.15 part.
In the above-mentioned timber floor using organic silicon modified polyurethane adhesive, described adhesive is by weight by following
Raw material is made:
Methyl diphenylene diisocyanate 13 parts,
Hydroxyl-terminated injecting two methyl siloxane 5.5 parts,
Polytetrahydrofuran diol 35 parts,
Diisooctyl phthalate 20 parts,
Dabco33-LV 0.12 part,
DF-520 1.5 parts,
P-Methyl benzenesulfonyl isocyanate 0.12 part,
Gamma-aminopropyl-triethoxy-silane 0.15 part,
3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate 0.08 part.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, described polyisocyanates is selected from diphenyl
In methane diisocyanate, toluene di-isocyanate(TDI), hexamethylene diisocyanate, polyphenyl polymethylene polyisocyanates
One or more.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, described is selected from 100-containing active hydrogen silicone oil
One or more in the hydroxyl-terminated injecting two methyl siloxane of 20000cP, terminal hydroxy group phenyl silicone oil, Amino End Group silicone oil.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, described polyhydric alcohol is selected from mean molecule quantity
At the polytetrahydrofuran diol of 1000-4000, polyoxypropyleneglycol, oxolane-ethylene oxide copolymer glycols, poly-three methylenes
One or more in base ether glycol, 10PE27 glycol；Described plasticizer is selected from phthalate, right
One or more in the many esters of gallic acid of Phthalates, benzene.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, described catalyst selected from triethanolamine,
One or more in triethylenediamine, dibutyl tin laurate, Dabco33-LV, zinc naphthenate.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, described defoamer is selected from DF-520, DF-
530, one or more in DF-899, DF-834；Described deicer is selected from triethyl orthoformate, to Methyl benzenesulfonyl isocyanide
One or more in acid esters.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, described coupling agent is by γ-aminopropyl three
Ethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane
In one or more；Described antioxidant is selected from 2,2'-ethylenedioxybis(ethanol). pair-[3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propanoic acid
Ester], 3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate, the antioxygen such as 3,5-di-t-butyl-4 different monooctyl ester of hydroxy phenylpropionic acid
One or more in agent.
In the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, the preparation method of described adhesive includes
Following steps:
1) polyhydric alcohol dehydration: weigh polyhydric alcohol according to weight ratio and put in reactor, be stirred and heated to 80-100 DEG C, take out
Vacuum dehydration processes 3-4 hour；
2) premixed systems preparation: to being cooled in the polyhydric alcohol of room temperature according to weight ratio addition defoamer after processed,
It is uniformly mixing to obtain premixed systems；
3) preparation of the isocyanate groups terminated polyurethane prepolymers containing organosilicon: add containing living according to weight ratio in polyisocyanates
Sprinkling hydrogen silicone oil, be stirred and heated to 80-90 DEG C, isothermal reaction to bubble-free is further continued for reaction 2-3 hour after producing, prepare and contain
The isocyanate groups terminated polyurethane prepolymers of machine silicon；
4) prepared by performed polymer: to step 2) obtained by premixed systems in add step 3) obtained by the end containing organosilicon different
Cyanate based prepolymers, is stirred and heated to 80-90 DEG C, and isothermal reaction to bubble-free is further continued for reaction 2-3 hour, system after producing
The performed polymer of organosilicon must be contained；
5) prepared by adhesive: is first according to weight ratio and adds in the performed polymer containing organosilicon, very by plasticizer, deicer
Stir 1-2 hour under empty condition；In mixed system, antioxidant, coupling agent and catalyst is added subsequently according to weight ratio,
Continue stirring 3 hours under vacuum condition, finally obtain finished product.
The heat treatment method of the timber floor of aforesaid employing organic silicon modified polyurethane adhesive, specification blank enters kiln, with
The heating rate of 1 degree Celsius per minute is warming up to 130 degrees Celsius, is now passed through overheated saturated steam, Control for Oxygen Content is existed
2%, constant temperature one hour, then it is warming up to 200 degrees Celsius with the heating rate of 1 degree Celsius per minute, constant temperature 2 hours, with per minute 1
Degree Celsius rate of temperature fall be down to 130 degrees Celsius, close overheated saturated steam, constant temperature half an hour, with 1 degree Celsius per minute
Rate of temperature fall is down to 80 degrees Celsius, constant temperature 1 hour, closes heating system, naturally cools to 40 degrees Celsius, shutdown, kiln discharge.
The present invention compares with prior art, and the present invention includes substrate, and the upper strata of substrate is pasted with epidermis, substrate through adhesive
Lower section is pasted with base plate through adhesive, and substrate is the finger-jointed plate pasted through adhesive by wooden unit.The adhesive of the present invention leads to
Cross rational component and proportioning, first by isocyanates with containing active hydrogen silicone oil (containing hydrogen silicone oil refers in particular to the silicone oil containing si-h bond,
But si-h bond torpescence, the reaction with isocyanates needs platinum catalyst.And the silicon Han active hydrogen, such as hydroxy silicon oil and amino
Silicone oil, does not has si-h bond, but the hydrogen activity of hydroxyl and amino is the highest, can react with isocyanates rapidly) pre-polymerization, rely on different
Reaction between active hydrogen in cyanic acid ester group and silicone oil, it is achieved the introducing of silicone segments, obtain containing organosilicon is isocyanate terminated
Based prepolymers；Then by prepolymer and polymerization, organic-silicon-modified adhesive for polyurethane, silicone molecules are finally given
The introducing of segment is effectively increased the resistance to water of adhesive for polyurethane.As can be seen here, the present invention has superior thermostability, water-fast
Property, widen the application of adhesive for polyurethane, the industrialized production of high performance polyurethane adhesive and in national industry
In extensively application serve positive impetus.Further, applicant's also heat treatment method to timber floor has been made to change
Entering, the heat treatment method after improvement further increases the mechanical property of product.
Detailed description of the invention
Embodiment 1: a kind of timber floor using organic silicon modified polyurethane adhesive, including substrate, the upper strata warp of substrate
Adhesive is pasted with epidermis, is pasted with base plate through adhesive below substrate, and substrate is the finger pasted through adhesive by wooden unit
Fishplate bar；Described adhesive is prepared by the raw materials in: polytetrahydrofuran diol (molecular weight 2000) 40 parts, diphenyl
Methane diisocyanate 8.7 parts, hydroxyl-terminated injecting two methyl siloxane 10 parts, DF-520 are 1.1 parts, Dabco33-LV is 0.08
Part, diisooctyl phthalate 20 parts, p-Methyl benzenesulfonyl isocyanate 0.05 part, gamma-aminopropyl-triethoxy-silane
0.05 part, 3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate 0.05 part.
Concrete preparation process is:
1) weigh in the reactor that the polytetrahydrofuran diol that 400g molecular weight is 2000 puts into 1L, be stirred and heated to
100 DEG C, evacuation processed 4 hours；
2) putting into 11gDF-520 successively to being cooled to after processed in the polytetrahydrofuran diol of room temperature, machinery stirs
Mix and uniformly obtain premixed systems；
3) in 87g methyl diphenylene diisocyanate, add hydroxyl-terminated injecting two methyl siloxane 100g, stir and heat
To 80-90 DEG C, isothermal reaction to bubble-free is further continued for reaction 2-3 hour after producing, prepare the terminal isocyanate group containing organosilicon
Prepolymer；
4) by step 3) in the obtained isocyanate groups terminated polyurethane prepolymers containing organosilicon all join step 2) made
In the premixed systems obtained, being stirred and heated to 90 DEG C, isothermal reaction to bubble-free is further continued for reacting 2 hours after producing, and prepares and contains
The performed polymer of machine silicon；
5) in obtained performed polymer, diisooctyl phthalate 200g it is sequentially added into, to Methyl benzenesulfonyl Carbimide.
Ester 5g, under vacuum stirring 2 hours；With backward mixed system adds Dabco33-LV8g, gamma-aminopropyl-triethoxy
Silane 5g, 3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate 5g, continue stirring 3 hours under vacuum；Finally
Obtain organic-silicon-modified adhesive for polyurethane.
Adhesive heat resisting temperature prepared by this example can bring up to 160 degrees centigrade after tested, contact angle after solidification
More than 90 °.
The preparation method of timber floor can use the preparation section of routine, first mutually pastes with little batten and obtains substrate, substrate
Surface and bottom surface coating adhesive, then paste upper dash board and base plate.
Using the heat treatment method of the timber floor of organic silicon modified polyurethane adhesive, specification blank enters kiln, with per minute 1
Degree Celsius heating rate be warming up to 130 degrees Celsius, be now passed through overheated saturated steam, by Control for Oxygen Content 2%, constant temperature
One hour, then it is warming up to 200 degrees Celsius with the heating rate of 1 degree Celsius per minute, constant temperature 2 hours, with 1 degree Celsius per minute
Rate of temperature fall is down to 130 degrees Celsius, closes overheated saturated steam, constant temperature half an hour, with the rate of temperature fall of 1 degree Celsius per minute
It is down to 80 degrees Celsius, constant temperature 1 hour, close heating system, naturally cool to 40 degrees Celsius, shutdown, kiln discharge.
Embodiment 2: a kind of timber floor using organic silicon modified polyurethane adhesive, including substrate, the upper strata warp of substrate
Adhesive is pasted with epidermis, is pasted with base plate through adhesive below substrate, and substrate is the finger pasted through adhesive by wooden unit
Fishplate bar；Described adhesive is prepared by the raw materials in: polytetrahydrofuran diol (molecular weight 3000) 60 parts, diphenyl
Methane diisocyanate 8.7 parts, Amino End Group silicone oil 4 parts, DF-520 are 0.6 part, Dabco33-LV is 0.08 part, phthalic acid
Di-isooctyl 20 parts, p-Methyl benzenesulfonyl isocyanate 0.05 part, gamma-aminopropyl-triethoxy-silane 0.05 part, 3,5-bis-uncle
Butyl-4 hydroxy-phenylpropionic acid ten caprylate 0.05 part.
Concrete preparation process is:
1) weigh in the reactor that the polytetrahydrofuran diol that 600g molecular weight is 3000 puts into 2L, be stirred and heated to
100 DEG C, evacuation processed 5 hours；
2) 6gDF-520, mechanical agitation are put into successively to being cooled to after processed in the polytetrahydrofuran diol of room temperature
Uniformly obtain premixed systems；
3) in 87g methyl diphenylene diisocyanate, add Amino End Group silicone oil 40g, be stirred and heated to 80-90 DEG C, permanent
Temperature reaction is further continued for reaction 2-3 hour after producing to bubble-free, prepares the isocyanate groups terminated polyurethane prepolymers containing organosilicon；
4) by step 3) in the obtained isocyanate groups terminated polyurethane prepolymers containing organosilicon all join step 2) made
In the premixed systems obtained, being stirred and heated to 90 DEG C, isothermal reaction to bubble-free is further continued for reacting 2 hours after producing, and prepares and contains
The performed polymer of machine silicon；
5) in obtained performed polymer, diisooctyl phthalate 200g it is sequentially added into, to Methyl benzenesulfonyl Carbimide.
Ester 5g, under vacuum stirring 2 hours；With backward mixed system adds Dabco33-LV8g, gamma-aminopropyl-triethoxy
Silane 5g, 3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate 5g, continue stirring 3 hours under vacuum；Finally
Obtain organic silicon modified polyurethane adhesive.
Adhesive heat resisting temperature prepared by this example can bring up to 160 degrees centigrade after tested, contact angle after solidification
More than 90 °
Using the heat treatment method of the timber floor of organic silicon modified polyurethane adhesive, specification blank enters kiln, with per minute 1
Degree Celsius heating rate be warming up to 130 degrees Celsius, be now passed through overheated saturated steam, by Control for Oxygen Content 2%, constant temperature
One hour, then it is warming up to 200 degrees Celsius with the heating rate of 1 degree Celsius per minute, constant temperature 2 hours, with 1 degree Celsius per minute
Rate of temperature fall is down to 130 degrees Celsius, closes overheated saturated steam, constant temperature half an hour, with the rate of temperature fall of 1 degree Celsius per minute
It is down to 80 degrees Celsius, constant temperature 1 hour, close heating system, naturally cool to 40 degrees Celsius, shutdown, kiln discharge.
Embodiment 3: a kind of timber floor using organic silicon modified polyurethane adhesive, including substrate, the upper strata warp of substrate
Adhesive is pasted with epidermis, is pasted with base plate through adhesive below substrate, and substrate is the finger pasted through adhesive by wooden unit
Fishplate bar；Described adhesive is prepared by the raw materials in: methyl diphenylene diisocyanate 13 parts, the poly-diformazan of terminal hydroxy group
Radical siloxane 5.5 parts, polytetrahydrofuran diol 35 parts, diisooctyl phthalate 20 parts, Dabco33-LV 0.12 part, DF-
520 1.5 parts, p-Methyl benzenesulfonyl isocyanate 0.12 part, gamma-aminopropyl-triethoxy-silane 0.15 part, 3,5-bis-tertiary fourths
Base-4 hydroxy-phenylpropionic acid ten caprylate 0.08 part.
Concrete preparation process is:
1) weigh in the reactor that the polytetrahydrofuran diol that molecular weight is 3000 is put into, be stirred and heated to 100 DEG C,
Evacuation processed 4 hours；
2) putting into DF-520 successively to being cooled to after processed in the polytetrahydrofuran diol of room temperature, mechanical agitation is equal
Even obtain premixed systems；
3) in methyl diphenylene diisocyanate, add hydroxyl-terminated injecting two methyl siloxane, be stirred and heated to 80-90
DEG C, isothermal reaction to bubble-free is further continued for reaction 2-3 hour after producing, prepare the isocyanate groups terminated polyurethane prepolymers containing organosilicon；
4) by step 3) in the obtained isocyanate groups terminated polyurethane prepolymers containing organosilicon all join step 2) made
In the premixed systems obtained, being stirred and heated to 90 DEG C, isothermal reaction to bubble-free is further continued for reacting 2 hours after producing, and prepares and contains
The performed polymer of machine silicon；
5) in obtained performed polymer, diisooctyl phthalate, p-Methyl benzenesulfonyl isocyanate it are sequentially added into,
Stirring 2 hours under vacuum；With in backward mixed system add Dabco33-LV, gamma-aminopropyl-triethoxy-silane, 3,
5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate, continues stirring 3 hours under vacuum；Finally obtain organosilicon to change
The adhesive for polyurethane of property.
Adhesive heat resisting temperature prepared by this example can bring up to 180 degrees centigrade after tested, contact angle after solidification
More than 90 °.
Using the heat treatment method of the timber floor of organic silicon modified polyurethane adhesive, specification blank enters kiln, with per minute 1
Degree Celsius heating rate be warming up to 130 degrees Celsius, be now passed through overheated saturated steam, by Control for Oxygen Content 2%, constant temperature
One hour, then it is warming up to 200 degrees Celsius with the heating rate of 1 degree Celsius per minute, constant temperature 2 hours, with 1 degree Celsius per minute
Rate of temperature fall is down to 130 degrees Celsius, closes overheated saturated steam, constant temperature half an hour, with the rate of temperature fall of 1 degree Celsius per minute
It is down to 80 degrees Celsius, constant temperature 1 hour, close heating system, naturally cool to 40 degrees Celsius, shutdown, kiln discharge.
Embodiment 4: gluing power comprehensive performance test.
Shear strength is pressed GB7124-86 and is measured；
Peel strength is pressed GB/T7122-1996 and is measured.
The timber floor of Example 1 and 2, then take the row timber floor prepared of adhesive for polyurethane commonly used in the trade as a comparison
Group, a point cold curing measures its shear strength and peel strength in 24 hours, 3 days and 10 days, is shown in Table 1.
Table 1 timber floor adhesive test
As it can be seen from table 1 embodiment 1 and embodiment 2 are under 25 DEG C of environment, shear strength is substantially better than contrast groups,
150 DEG C of environment down cut intensity are also significantly better than contrast groups, effect highly significant.And embodiment 1 and the peel strength of embodiment 2
Also contrast groups it is significantly better than.As can be seen here, the present invention not only has superior stickup performance, and the present invention effectively improves resistance to
High-temperature behavior, has widened use temperature range.
Claims (10)
1. use the timber floor of organic silicon modified polyurethane adhesive, it is characterised in that: including substrate, the upper strata of substrate is through gluing
Agent is pasted with epidermis, is pasted with base plate through adhesive below substrate, and substrate is the finger-jointed plate pasted through adhesive by wooden unit；
Described adhesive is made up of following raw materials according by weight:
Polyisocyanates 5-20 part,
Containing active hydrogen silicone oil 1-20 part,
Polyhydric alcohol 30-50 part,
Plasticizer 10-30 part,
Catalyst 0.05-0.20 part,
Defoamer 0.5-3 part,
Deicer 0.02-0.20 part,
Coupling agent 0.02-0.30 part,
Antioxidant 0.02-0.15 part.
The timber floor of employing organic silicon modified polyurethane adhesive the most according to claim 1 and 2, it is characterised in that: institute
The adhesive stated is made up of following raw materials according by weight:
Methyl diphenylene diisocyanate 13 parts,
Hydroxyl-terminated injecting two methyl siloxane 5.5 parts,
Polytetrahydrofuran diol 35 parts,
Diisooctyl phthalate 20 parts,
Dabco33-LV 0.12 part,
DF-520 1.5 parts,
P-Methyl benzenesulfonyl isocyanate 0.12 part,
Gamma-aminopropyl-triethoxy-silane 0.15 part,
3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate 0.08 part.
The timber floor of employing organic silicon modified polyurethane adhesive the most according to claim 1 and 2, it is characterised in that: institute
The polyisocyanates stated is selected from methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), hexamethylene diisocyanate, many benzene
One or more in the methylene polyisocyanates of Quito.
The timber floor of employing organic silicon modified polyurethane adhesive the most according to claim 1 and 2, it is characterised in that: institute
That states is selected from the hydroxyl-terminated injecting two methyl siloxane of 100-20000cP, terminal hydroxy group phenyl silicone oil, Amino End Group silicon containing active hydrogen silicone oil
One or more in oil.
The timber floor of employing organic silicon modified polyurethane adhesive the most according to claim 1 and 2, it is characterised in that: institute
The polyhydric alcohol stated selected from mean molecule quantity the polytetrahydrofuran diol of 1000-4000, polyoxypropyleneglycol, oxolane-
One or more in ethylene oxide copolymer glycols, polytrimethylene ether glycol, 10PE27 glycol；Described increasing
Mould one or more in phthalate, terephthalic acid ester, the many esters of gallic acid of benzene of agent.
The timber floor of employing organic silicon modified polyurethane adhesive the most according to claim 1 and 2, it is characterised in that: institute
The catalyst stated is in triethanolamine, triethylenediamine, dibutyl tin laurate, Dabco33-LV, zinc naphthenate
One or more.
The timber floor of employing organic silicon modified polyurethane adhesive the most according to claim 1 and 2, it is characterised in that: institute
One or more in DF-520, DF-530, DF-899, DF-834 of the defoamer stated；Described deicer is selected from primitive nail
One or more in triethylenetetraminehexaacetic acid ester, p-Methyl benzenesulfonyl isocyanate.
8., according to the timber floor using organic silicon modified polyurethane adhesive described in any one of claim 1-7, its feature exists
In: described coupling agent is by gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(first
Base acryloyl-oxy) one or more in propyl trimethoxy silicane；Described antioxidant is selected from 2,2'-ethylenedioxybis(ethanol). pair-[3-(uncle 3-
Butyl-4-hydroxy-5-methyl base phenyl) propionic ester], 3,5-di-t-butyl-4 hydroxy-phenylpropionic acid ten caprylate, 3,5-bis-uncle
One or more in the antioxidants such as butyl-4 different monooctyl ester of hydroxy phenylpropionic acid.
9., according to the timber floor using organic silicon modified polyurethane adhesive described in any one of claim 1-8, its feature exists
In: the preparation method of described adhesive comprises the following steps:
1) polyhydric alcohol dehydration: weigh polyhydric alcohol according to weight ratio and put in reactor, be stirred and heated to 80-100 DEG C, evacuation
Processed 3-4 hour；
2) premixed systems preparation: to being cooled to after processed in the polyhydric alcohol of room temperature according to weight ratio addition defoamer, stirring
Uniformly obtain premixed systems；
3) preparation of the isocyanate groups terminated polyurethane prepolymers containing organosilicon: add containing active hydrogen according to weight ratio in polyisocyanates
Silicone oil, is stirred and heated to 80-90 DEG C, and isothermal reaction to bubble-free is further continued for reaction 2-3 hour after producing, prepare containing organosilicon
Isocyanate groups terminated polyurethane prepolymers；
4) prepared by performed polymer: to step 2) obtained by premixed systems in add step 3) obtained by the end Carbimide. containing organosilicon
Ester group prepolymer, is stirred and heated to 80-90 DEG C, and isothermal reaction to bubble-free is further continued for reaction 2-3 hour after producing, prepare and contain
The performed polymer of organosilicon；
5) prepared by adhesive: is first according to weight ratio and adds in the performed polymer containing organosilicon, at vacuum bar by plasticizer, deicer
Stir 1-2 hour under part；In mixed system, antioxidant, coupling agent and catalyst is added subsequently, in vacuum according to weight ratio
Under the conditions of continue stirring 3 hours, finally obtain finished product.
10. according to the heat treatment method of the timber floor using organic silicon modified polyurethane adhesive described in claim 1-9, its
It is characterised by: specification blank enters kiln, is warming up to 130 degrees Celsius with the heating rate of 1 degree Celsius per minute, be now passed through overheated full
And steam, by Control for Oxygen Content 2%, constant temperature one hour, then be warming up to 200 with the heating rate of 1 degree Celsius per minute and take the photograph
Family name's degree, constant temperature 2 hours, it is down to 130 degrees Celsius with the rate of temperature fall of 1 degree Celsius per minute, closes overheated saturated steam, constant temperature
Half an hour, it is down to 80 degrees Celsius with the rate of temperature fall of 1 degree Celsius per minute, constant temperature 1 hour, close heating system, natural cooling
To 40 degrees Celsius, shutdown, kiln discharge.
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| CN201610584800.1A CN106189997A (en) | 2016-07-22 | 2016-07-22 | Use timber floor and the heat treatment method thereof of organic silicon modified polyurethane adhesive |
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| CN201610584800.1A CN106189997A (en) | 2016-07-22 | 2016-07-22 | Use timber floor and the heat treatment method thereof of organic silicon modified polyurethane adhesive |
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| CN105860912A (en) * | 2016-04-14 | 2016-08-17 | 久盛地板有限公司 | Polyimide modified polyurethane adhesive and preparing method thereof |
| CN106977687A (en) * | 2017-04-27 | 2017-07-25 | 久盛地板有限公司 | Environment-protecting polyurethane antibacterial adhesive and preparation method thereof |
| CN108504321A (en) * | 2018-05-07 | 2018-09-07 | 安吉祥力胶粘剂有限公司 | A kind of organic silicon polyurethane adhesive and preparation method thereof |
| CN109082259A (en) * | 2018-07-30 | 2018-12-25 | 苏州市回天科技有限公司 | A kind of insulation adhesive and preparation method thereof |
| CN115368866A (en) * | 2022-09-23 | 2022-11-22 | 山东尚正新材料科技股份有限公司 | High-strength polyurethane adhesive and preparation method thereof |
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| CN109082259A (en) * | 2018-07-30 | 2018-12-25 | 苏州市回天科技有限公司 | A kind of insulation adhesive and preparation method thereof |
| CN115368866A (en) * | 2022-09-23 | 2022-11-22 | 山东尚正新材料科技股份有限公司 | High-strength polyurethane adhesive and preparation method thereof |
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Application publication date: 20161207 |