CN111253899A - Industrial water washing resistant bright silver reflective fabric adhesive and preparation method thereof - Google Patents
Industrial water washing resistant bright silver reflective fabric adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN111253899A CN111253899A CN202010209096.8A CN202010209096A CN111253899A CN 111253899 A CN111253899 A CN 111253899A CN 202010209096 A CN202010209096 A CN 202010209096A CN 111253899 A CN111253899 A CN 111253899A
- Authority
- CN
- China
- Prior art keywords
- adhesive
- water washing
- industrial water
- parts
- silver reflective
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- 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
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
- C08G18/425—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids the polyols containing one or two ether 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to an adhesive for industrial water washing resistant bright silver reflective fabric and a preparation method thereof, wherein the adhesive is prepared by compounding polyurethane main body resin prepared by taking polyester and/or polyether glycol and isocyanate as raw materials, a coupling agent, a catalyst, an anti-hydrolysis auxiliary agent and a solvent, and comprises the following components in percentage by mass: 20-40% of polyester polyol; the molecular weight of the polyester polyol is as follows: 1000 to 3000 parts; 0-15% of polyether polyol; 3-5% of isocyanate; 50% -60% of a solvent; 0.4 to 2 percent of coupling agent; 0.01 to 0.1 percent of catalyst; the catalyst is as follows: one or a combination of bismuth isooctanoate and bismuth neodecanoate; 0.5% -2% of hydrolysis-resistant auxiliary agent, good bonding strength, flexible hand feeling, excellent hydrolysis resistance, simple process, energy conservation, environmental protection, strong initial adhesion and suitability for popularization.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an adhesive for industrial water washing resistant bright silver reflective cloth and a preparation method thereof, which are mainly applied to the field of polyurethane adhesives for industrial water washing resistant reflective cloth.
Background
In the prior art, an adhesive for reflective cloth mainly adopts acrylic resin system resin and polyurethane system resin, wherein the acrylic resin system is mainly used for reflective products with relatively mild washing conditions, and the polyurethane system resin is used for reflective products with more severe washing conditions, especially for industrial washing-resistant bright silver cloth, and the products require no obvious damage to the appearance of the washed products and good preservation of the reflectivity after being washed for 100 times/2 h in 90 ℃ hot water containing washing powder;
for example: the adhesive special for the light reflecting material containing polyether polyol polyurethane, invented by U.S. 3M company disclosed in patent No. CN95196332.5, is excellent in water washing resistance, and the product is good in flexible hand feeling, but in practical application, the initial adhesion of the product is poor;
in order to overcome the not enough of just viscous force poor, a compound glue of polyurethane for reflecting material appears in prior art, this glue is mostly polyester polyurethane product, this kind of product is used for bonding fabric and reflecting material, can make the clothing have superstrong high temperature water washing resistance after the bonding, the product reflection of light degree is preserved well after the washing, but under harsh condition, the adhesive linkage sclerosis after the washing, there is the phenomenon of breaking away between messenger's adhesive linkage and the fabric, make the whole outward appearance of product incomplete.
Disclosure of Invention
Aiming at the defect that the bright silver reflective cloth compounded by the polyurethane adhesive has poor washability under the industrial washing condition, the invention greatly enhances the washing tolerance under the harsh condition by optimized process design and scientific component proportion, and has the advantages of simple process, energy conservation, environmental protection, strong initial adhesion and suitability for popularization.
In order to achieve the purpose, the invention provides an adhesive for industrial water washing resistant bright silver reflective cloth and a preparation method thereof, wherein the adhesive comprises the following components in parts by weight:
an adhesive for industrial water washing resistant bright silver reflective cloth comprises the following components in percentage by mass:
①, 20 to 40 percent of polyester polyol, wherein the molecular weight of the polyester polyol is 1000 to 3000;
as an illustration, the polyester polyol employs: sebacic acid, isophthalic acid, adipic acid, ethylene glycol, diethylene glycol and neopentyl glycol are used as raw materials, tetrabutyl titanate is used as a catalyst, triphenyl phosphite is used as an antioxidant, and the components are subjected to esterification and polycondensation reaction to obtain the polyester prepolymer; the raw materials comprise the following components in percentage by weight: 15-35 parts of sebacic acid, 12-30 parts of isophthalic acid, 3-10 parts of adipic acid, 8-15 parts of ethylene glycol, 7-18 parts of diethylene glycol, 20-30 parts of neopentyl glycol, 0.01-0.03 part of tetra-n-butyl titanate and 0.04-0.06 part of triphenyl phosphite;
②, 0-15% of polyether polyol;
as an illustration, the polyether polyol is: polytetrahydrofuran ether with the molecular weight of 1000-3000;
③, 3-5% of isocyanate;
as an illustration, the isocyanate is: one or a combination of MDI, TDI, IPDI and PAPI;
④ solvent 50% -60%;
as an illustration, the solvent is: one or a combination of toluene, xylene, ethyl acetate and dimethyl carbonate;
⑤ coupling agent 0.4% -2%;
as an illustration, the coupling agent is: one or a combination of glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane and gamma-aminopropyltriethoxysilane;
⑥ catalyst 0.01% -0.1%;
as an illustration, the catalyst is: one or a combination of bismuth isooctanoate and bismuth neodecanoate;
⑦ hydrolysis resistant assistant 0.5% -2%.
The adhesive is prepared by compounding polyurethane main body resin prepared by reacting polyester/polyether polyol and isocyanate as raw materials with a coupling agent, a catalyst, an anti-hydrolysis auxiliary agent and a solvent, wherein the solid content of the product is 40-50%, and the viscosity of the product is 5000-8000mPa □ s;
a preparation method of an adhesive for industrial water washing resistant bright silver reflective fabric comprises the following steps:
step one, heating a certain amount of polyester polyol and/or polyether polyol to 120 ℃, stirring and mixing uniformly, simultaneously carrying out reduced pressure dehydration for 2h, and then cooling to 60 ℃;
as an illustration, the decompression dehydration process requires that the vacuum degree is more than or equal to 0.1 MPa;
as an illustration, the polyether polyol is: polytetrahydrofuran ether with molecular weight of 1000-3000, and commercial products such as: PTMEG1000, PTMEG2000, PTMEG3000, and the like;
further, the preparation method of the polyester polyol comprises the following steps:
①, primary esterification, namely adding sebacic acid, isophthalic acid, adipic acid, ethylene glycol, diethylene glycol and neopentyl glycol into a polyester reaction kettle for one time, heating to 210-230 ℃, and reacting for 2-4 hours to complete the primary esterification, wherein the acid value of the primary esterification is less than or equal to 20mg KOH/g;
② polycondensation reaction, wherein after the primary esterification is finished, the polyester reaction kettle is vacuumized and is pre-vacuumized for 1h respectively according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, the kettle temperature of the polyester reaction kettle is controlled to be 225-230 ℃, then long-time vacuum pumping operation is carried out, the vacuum degree is-0.10 MPa, the long-time vacuum pumping operation is carried out, the distillate accounts for 4-7 h of the total weight of the raw materials, the hydroxyl value of the polyester polyol is 37-56 mg KOH/g, and the relative molecular weight is 2000-3000 g/mol;
secondly, under the protection of nitrogen, adding a catalyst, a solvent and isocyanate into the reaction system in the first step, reacting for 3 hours at the temperature of 85-95 ℃, and cooling to below 60 ℃;
as an illustration, the isocyanate is: one or a combination of MDI, TDI, IPDI and PAPI;
as an illustration, the catalyst is: one or a combination of bismuth isooctanoate and bismuth neodecanoate;
as an illustration, the solvent is: one or a combination of toluene, xylene, ethyl acetate and dimethyl carbonate;
and step three, adding a coupling agent and an anti-hydrolysis auxiliary agent to obtain the industrial washing-resistant bright silver reflective fabric adhesive.
As an illustration, the coupling agent is: one or a combination of glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane and gamma-aminopropyltriethoxysilane;
as an illustration, the anti-hydrolysis auxiliary agent is monocarbodiimide or polycarbodiimide, and is commercially available as HyMax 1010, Stabolizer 7000F and the like.
Has the advantages that:
the polyurethane adhesive has better bonding strength to polar materials, the adhesive prepared by adopting a special process has the advantages of both polyester polyurethane and polyether polyurethane, and the polyether polyurethane has flexible hand feeling, excellent hydrolysis resistance, excellent bonding performance to the polyester polyurethane and excellent bonding performance to the polar materials;
after common polyester polyol and polyether polyol are mixed, the system is incompatible, the appearance of an adhesive system is poor, and the bonding effect is poor, and a large amount of polyester polyol and polyether polyol are analyzed, screened, combined and tested, so that the two systems adopted in the patent can be well compatible in the system, and the two polyols are organically combined in a point manner;
in addition, the added coupling agent can form a new interface layer on the bonding layer and the bonding interface of the glass beads, and the effect of enhancing the interface bonding is achieved.
Detailed Description
The following is a detailed description of a preferred embodiment of the present invention, an adhesive for industrial water washing resistant bright silver reflective cloth and a preparation method thereof, wherein:
an adhesive for industrial water washing resistant bright silver reflective cloth comprises the following components in percentage by mass:
①, 20 to 40 percent of polyester polyol, wherein the molecular weight of the polyester polyol is 1000 to 3000;
as an illustration, the polyester polyol employs: sebacic acid, isophthalic acid, adipic acid, ethylene glycol, diethylene glycol and neopentyl glycol are used as raw materials, tetrabutyl titanate is used as a catalyst, triphenyl phosphite is used as an antioxidant, and the components are subjected to esterification and polycondensation reaction to obtain the polyester prepolymer; the raw materials comprise the following components in percentage by weight: 15-35 parts of sebacic acid, 12-30 parts of isophthalic acid, 3-10 parts of adipic acid, 8-15 parts of ethylene glycol, 7-18 parts of diethylene glycol, 20-30 parts of neopentyl glycol, 0.01-0.03 part of tetra-n-butyl titanate and 0.04-0.06 part of triphenyl phosphite;
②, 0-15% of polyether polyol;
as an illustration, the polyether polyol is: polytetrahydrofuran ether with the molecular weight of 1000-3000;
③, 3-5% of isocyanate;
as an illustration, the isocyanate is: one or a combination of MDI, TDI, IPDI and PAPI;
④ solvent 50% -60%;
as an illustration, the solvent is: one or a combination of toluene, xylene, ethyl acetate and dimethyl carbonate;
⑤ coupling agent 0.4% -2%;
as an illustration, the coupling agent is: one or a combination of glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane and gamma-aminopropyltriethoxysilane;
⑥ catalyst 0.01% -0.1%;
as an illustration, the catalyst is: one or a combination of bismuth isooctanoate and bismuth neodecanoate;
⑦ hydrolysis resistant assistant 0.5% -2%.
The adhesive is prepared by compounding polyurethane main body resin prepared by reacting polyester/polyether polyol and isocyanate as raw materials with a coupling agent, a catalyst, an anti-hydrolysis auxiliary agent and a solvent, wherein the solid content of the product is 40-50%, and the viscosity of the product is 5000-8000mPa □ s;
a preparation method of an adhesive for industrial water washing resistant bright silver reflective fabric comprises the following steps:
step one, heating a certain amount of polyester polyol and/or polyether polyol to 120 ℃, stirring and mixing uniformly, simultaneously carrying out reduced pressure dehydration for 2h, and then cooling to 60 ℃;
as an illustration, the decompression dehydration process requires that the vacuum degree is more than or equal to 0.1 MPa;
as an illustration, the polyether polyol is: polytetrahydrofuran ether with molecular weight of 1000-3000, and commercial products such as: PTMEG1000, PTMEG2000, PTMEG3000, and the like;
further, the preparation method of the polyester polyol comprises the following steps:
①, primary esterification, namely adding sebacic acid, isophthalic acid, adipic acid, ethylene glycol, diethylene glycol and neopentyl glycol into a polyester reaction kettle for one time, heating to 210-230 ℃, and reacting for 2-4 hours to complete the primary esterification, wherein the acid value of the primary esterification is less than or equal to 20mg KOH/g;
② polycondensation reaction, wherein after the primary esterification is finished, the polyester reaction kettle is vacuumized and is pre-vacuumized for 1h respectively according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, the kettle temperature of the polyester reaction kettle is controlled to be 225-230 ℃, then long-time vacuum pumping operation is carried out, the vacuum degree is-0.10 MPa, the long-time vacuum pumping operation is carried out, the distillate accounts for 4-7 h of the total weight of the raw materials, the hydroxyl value of the polyester polyol is 37-56 mg KOH/g, and the relative molecular weight is 2000-3000 g/mol;
secondly, under the protection of nitrogen, adding a catalyst, a solvent and isocyanate into the reaction system in the first step, reacting for 3 hours at the temperature of 85-95 ℃, and cooling to below 60 ℃;
as an illustration, the isocyanate is: one or a combination of MDI, TDI, IPDI and PAPI;
as an illustration, the catalyst is: one or a combination of bismuth isooctanoate and bismuth neodecanoate;
as an illustration, the solvent is: one or a combination of toluene, xylene, ethyl acetate and dimethyl carbonate;
and step three, adding a coupling agent and an anti-hydrolysis auxiliary agent to obtain the industrial washing-resistant bright silver reflective fabric adhesive.
As an illustration, the coupling agent is: one or a combination of glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane and gamma-aminopropyltriethoxysilane;
as an illustration, the anti-hydrolysis auxiliary agent is monocarbodiimide or polycarbodiimide, and is commercially available as HyMax 1010, Stabolizer 7000F and the like.
In order to better explain the design principle of the present invention, a brief description will be given by way of embodiments;
the first embodiment is as follows: a preparation method of an adhesive for industrial water washing resistant bright silver reflective fabric comprises the following steps:
step one, preparing polyester polyol (the raw materials are calculated according to mass percentage): adding the following components into a polyester reaction kettle: 29 parts by mass of sebacic acid, 25 parts by mass of isophthalic acid, 4 parts by mass of adipic acid, 8 parts by mass of ethylene glycol, 9 parts by mass of dihexylene glycol, 25 parts by mass of neopentyl glycol, 0.02 part by mass of tetra-n-butyl titanate and 0.04 part by mass of triphenyl phosphite, fully and uniformly stirring, heating to 210-230 ℃, reacting for 4 hours, distilling off 11.8 parts by mass of water, and measuring the acid value to be 17.9mg KOH/g after the esterification is finished;
after the esterification is finished, vacuumizing the polyester kettle to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, and pre-vacuumizing for 1h in sequence, wherein the kettle temperature is controlled at 225-; after the pre-pumping is finished, performing long-time vacuum pumping operation, wherein the vacuum degree reaches-0.1 MPa, the long-time vacuum pumping operation lasts for 6 hours, and the mass part of distilled alcohol is 5.2 parts; the hydroxyl value of the finally prepared polyester resin is 48.8 mgKOH/g;
step two, under the protection of nitrogen, heating 35 parts by mass of polyester polyol and 5 parts by mass of PTMEG1000 polyether polyol in the step one to 120 ℃, stirring and mixing uniformly, simultaneously carrying out reduced pressure dehydration for 2h (the vacuum degree is more than or equal to 0.1MPa), and then cooling to 60 ℃; adding 0.01 part by mass of bismuth isooctanoate, 4 parts by mass of isocyanate MDI and 54 parts by mass of ethyl acetate, reacting for 3 hours at 85-95 ℃, cooling to below 40 ℃, and sampling to measure the viscosity to be 5800mPa □ s;
and step three, adding 1 part by mass of hydrolysis-resistant additive HyMax 1010 and 1 part by mass of coupling agent KH550, and stirring for 30min to obtain the adhesive for the industrial water-washing-resistant bright silver cloth.
Example two: a preparation method of an adhesive for industrial water washing resistant bright silver reflective fabric comprises the following steps:
step one, preparing polyester polyol (the raw materials are calculated according to mass percentage): adding 26 parts by mass of sebacic acid, 19 parts by mass of isophthalic acid, 14 parts by mass of adipic acid, 10 parts by mass of ethylene glycol, 9 parts by mass of dihexylene glycol, 22 parts by mass of neopentyl glycol, 0.02 part by mass of tetra-n-butyl titanate and 0.04 part by mass of triphenyl phosphite into a polyester reaction kettle, fully and uniformly stirring, heating to 210-230 ℃, reacting for 4 hours, distilling off 13.4 parts by mass of water, and measuring the acid value to be 16.5mg KOH/g after the esterification is finished; after the esterification is finished, vacuumizing the polyester kettle to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, and pre-vacuumizing for 1h in sequence, wherein the kettle temperature is controlled at 225-; after the pre-pumping is finished, performing long-time vacuum pumping operation, wherein the vacuum degree reaches-0.1 MPa, the long-time vacuum pumping operation lasts for 6 hours, and the mass part of distilled alcohol is 5.4 parts; the hydroxyl value of the finally prepared polyester resin is 54.3 mgKOH/g;
step two, under the protection of nitrogen, heating 30 parts by mass of polyester polyol and 8 parts by mass of PTMEG1000 polyether polyol in the step one to 120 ℃, stirring and mixing uniformly, simultaneously carrying out reduced pressure dehydration for 2h (the vacuum degree is more than or equal to 0.1MPa), then cooling to 60 ℃, adding 0.01 part by mass of bismuth isooctanoate, 5 parts by mass of isocyanate TDI and 56 parts by mass of dimethyl carbonate, reacting for 3h at the temperature of 85-95 ℃, cooling to below 40 ℃, and sampling and measuring the viscosity to 6200mPa □ s;
and step three, adding 0.8 part by mass of hydrolysis-resistant auxiliary agent HyMax 1010 and 1 part by mass of coupling agent KH560, and stirring for 30min to obtain the adhesive for the industrial water-washing-resistant bright silver cloth.
Example three: a preparation method of an adhesive for industrial water washing resistant bright silver reflective fabric comprises the following steps:
step one, preparing polyester polyol (the raw materials are calculated according to mass percentage): adding 24 parts by mass of sebacic acid, 18 parts by mass of isophthalic acid, 16 parts by mass of adipic acid, 10 parts by mass of ethylene glycol, 11 parts by mass of dihexylene glycol, 21 parts by mass of neopentyl glycol, 0.02 part by mass of tetra-n-butyl titanate and 0.04 part by mass of triphenyl phosphite into a polyester reaction kettle, fully and uniformly stirring, heating to 210-230 ℃, reacting for 4 hours, distilling off 12.5 parts by mass of water, and measuring the acid value to be 18.8mg KOH/g after the esterification is finished; after the esterification is finished, vacuumizing the polyester kettle to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, and pre-vacuumizing for 1h in sequence, wherein the kettle temperature is controlled at 225-; after the pre-pumping is finished, performing long-time vacuum pumping operation, wherein the vacuum degree reaches-0.1 MPa, the long-time vacuum pumping operation lasts for 6 hours, and the mass part of distilled alcohol is 6.8 parts; the hydroxyl value of the finally prepared polyester resin is 52.2 mgKOH/g;
step two, under the protection of nitrogen, heating 38 parts by mass of polyester polyol and 4 parts by mass of PTMEG3000 polyether polyol in the step one to 120 ℃, stirring and mixing uniformly, simultaneously decompressing and dehydrating for 2h (the vacuum degree is more than or equal to 0.1MPa), then cooling to 60 ℃, adding 0.02 part by mass of bismuth isooctanoate, 4 parts by mass of isocyanate TDI and 54 parts by mass of ethyl acetate, reacting for 3h at the temperature of 85-95 ℃, cooling to below 40 ℃, and sampling and measuring the viscosity to 6500mPa □ s;
and step three, adding 1.2 parts by mass of an anti-hydrolysis auxiliary agent HyMax 1010 and 0.8 part by mass of a coupling agent KH792, and stirring for 30min to obtain the adhesive for the industrial water washing resistant bright silver cloth.
After bright silver reflective fabrics were prepared according to the same process as in examples 1, 2 and 3, the fabrics were washed with water, the washing procedure was as described in patent No. CN95196332.5, the reflectivity was measured after washing, and the reflectance R was measured according to ASTM E810 as a standard test methodAThe results are shown in the following table:
| initial RA | After 100 cycles of washing RA | Degree of preservation | |
| Example 1 | 605 | 212 | 35.04％ |
| Example 2 | 613 | 220 | 35.89％ |
| Example 3 | 617 | 212 | 34.35％ |
| Comparative example | 608 | 208 | 34.2％ |
From the test results, the product of the invention has good industrial water washing resistance.
The polyurethane adhesive has better bonding strength to polar materials, the adhesive prepared by adopting a special process has the advantages of both polyester polyurethane and polyether polyurethane, and the polyether polyurethane has flexible hand feeling, excellent hydrolysis resistance, excellent bonding performance to the polyester polyurethane and excellent bonding performance to the polar materials; after common polyester polyol and polyether polyol are mixed, the system is incompatible, the appearance of an adhesive system is poor, and the bonding effect is poor, and a large amount of polyester polyol and polyether polyol are analyzed, screened, combined and tested, so that the two systems adopted in the patent can be well compatible in the system, and the two polyols are organically combined in a point manner; in addition, the added coupling agent can form a new interface layer on the bonding layer and the bonding interface of the glass beads, and the effect of enhancing the interface bonding is achieved.
The above embodiments are only preferred embodiments of the present invention, and it should be understood that the above embodiments are only for assisting understanding of the method and the core idea of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalents and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The adhesive for the industrial water washing resistant bright silver reflective cloth is characterized by comprising the following components in percentage by mass: 20-40% of polyester polyol; the molecular weight of the polyester polyol is as follows: 1000 to 3000 parts; 0-15% of polyether polyol; 3-5% of isocyanate; 50% -60% of a solvent; 0.4 to 2 percent of coupling agent; 0.01 to 0.1 percent of catalyst; the catalyst is as follows: one or a combination of bismuth isooctanoate and bismuth neodecanoate; 0.5 to 2 percent of hydrolysis-resistant auxiliary agent.
2. The adhesive for the industrial water washing-resistant bright silver reflective cloth as claimed in claim 1, wherein the polyester polyol adopts: sebacic acid, isophthalic acid, adipic acid, ethylene glycol, diethylene glycol and neopentyl glycol are used as raw materials, tetrabutyl titanate is used as a catalyst, triphenyl phosphite is used as an antioxidant, and the components are subjected to esterification and polycondensation reaction to obtain the polyester prepolymer; the raw materials comprise the following components in percentage by weight: 15-35 parts of sebacic acid, 12-30 parts of isophthalic acid, 3-10 parts of adipic acid, 8-15 parts of ethylene glycol, 7-18 parts of diethylene glycol, 20-30 parts of neopentyl glycol, 0.01-0.03 part of tetra-n-butyl titanate and 0.04-0.06 part of triphenyl phosphite.
3. The adhesive for the industrial water washing-resistant bright silver reflective cloth as claimed in claim 1, wherein the polyether polyol is: the molecular weight of the polytetrahydrofuran ether is 1000-3000.
4. The adhesive for the industrial water washing resistant bright silver reflective cloth according to claim 1, wherein the isocyanate is: one or a combination of MDI, TDI, IPDI and PAPI.
5. The adhesive for the industrial water washing resistant bright silver reflective cloth according to claim 1, wherein the solvent is: one or a combination of toluene, xylene, ethyl acetate and dimethyl carbonate.
6. The adhesive for the industrial water washing-resistant bright silver reflective cloth as claimed in claim 1, wherein the coupling agent is: one or the combination of glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane and gamma-aminopropyltriethoxysilane.
7. The adhesive for the industrial water washing-resistant bright silver reflective cloth is characterized by comprising the following components in percentage by weight: 40-50%, and the viscosity of the product is 5000-.
8. A preparation method of an adhesive for industrial water washing resistant bright silver reflective cloth is characterized by comprising the following steps:
step one, heating a certain amount of polyester polyol and/or polyether polyol to 120 ℃, stirring and mixing uniformly, simultaneously carrying out reduced pressure dehydration for 2h, and then cooling to 60 ℃;
the preparation method of the polyester polyol comprises the following steps:
primary esterification: adding sebacic acid, isophthalic acid, adipic acid, ethylene glycol, diethylene glycol and neopentyl glycol into a polyester reaction kettle for one time, heating to 210-230 ℃, reacting for 2-4 hours, and completing one-time esterification, wherein the acid value of the one-time esterification is less than or equal to 20 mgKOH/g;
and (3) polycondensation reaction: after the primary esterification is finished, vacuumizing a polyester reaction kettle for 1 hour according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester reaction kettle at 225-230 ℃, and then carrying out long vacuumizing operation, wherein the vacuum degree is-0.10 MPa, the long vacuumizing time is 5-7 hours, the distillate accounts for 4-7% of the total weight of the raw materials, the hydroxyl value of the final polyester polyol is 37-56 mg KOH/g, and the relative molecular weight is 2000-3000 g/mol;
secondly, under the protection of nitrogen, adding a catalyst, a solvent and isocyanate into the reaction system in the first step, reacting for 3 hours at the temperature of 85-95 ℃, and cooling to below 60 ℃;
and step three, adding a coupling agent and an anti-hydrolysis auxiliary agent to obtain the industrial washing-resistant bright silver reflective fabric adhesive.
9. The preparation method of the industrial water washing resistant bright silver reflective fabric adhesive according to claim 8, wherein the vacuum degree required by the decompression dehydration process is more than or equal to 0.1 MPa.
10. The preparation method of the industrial water washing resistant bright silver reflective fabric adhesive according to claim 8, wherein the hydrolysis resistance auxiliary agent is: monocarbodiimide or polycarbodiimide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010209096.8A CN111253899A (en) | 2020-03-23 | 2020-03-23 | Industrial water washing resistant bright silver reflective fabric adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010209096.8A CN111253899A (en) | 2020-03-23 | 2020-03-23 | Industrial water washing resistant bright silver reflective fabric adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111253899A true CN111253899A (en) | 2020-06-09 |
Family
ID=70942443
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010209096.8A Pending CN111253899A (en) | 2020-03-23 | 2020-03-23 | Industrial water washing resistant bright silver reflective fabric adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111253899A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110951419A (en) * | 2018-09-27 | 2020-04-03 | 江门市泰联新材料有限公司 | Hot melt adhesive |
| CN112297468A (en) * | 2020-10-13 | 2021-02-02 | 广东鸿驿聚氨酯科技有限公司 | Prepolymer and polyurethane seamless track for shot blasting machine and production process thereof |
| CN114957605A (en) * | 2022-07-04 | 2022-08-30 | 山东一诺威聚氨酯股份有限公司 | TPU (thermoplastic polyurethane) adhesive film material for traceless underwear and preparation method thereof |
| CN115181526A (en) * | 2021-08-30 | 2022-10-14 | 无锡博锦高分子研究发展有限公司 | Solvent-free washable reflective material adhesive and preparation method thereof |
| CN115584233A (en) * | 2022-02-22 | 2023-01-10 | 浙江星华反光材料有限公司 | Preparation process and application of high-toughness polyurethane adhesive |
| CN115820195A (en) * | 2022-08-15 | 2023-03-21 | 杭州星华反光材料股份有限公司 | Polyurethane glue for high-brightness reflective material and application thereof |
| CN115181526B (en) * | 2021-08-30 | 2024-05-31 | 无锡博锦高分子研究发展有限公司 | Solvent-free washable reflective material adhesive and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701141A (en) * | 2009-08-31 | 2010-05-05 | 北京高盟化工有限公司 | Preparation method of monocomponent moisturecured bonding agent for reflecting material |
| CN105295815A (en) * | 2015-11-11 | 2016-02-03 | 上海康达化工新材料股份有限公司 | Reactive polyurethane hot melt adhesive for reflective fabric and preparation method thereof |
| CN108165214A (en) * | 2018-01-03 | 2018-06-15 | 浙江恒劲树脂有限公司 | A kind of reflective preparation process for taking polyurethane resin composite glue |
-
2020
- 2020-03-23 CN CN202010209096.8A patent/CN111253899A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701141A (en) * | 2009-08-31 | 2010-05-05 | 北京高盟化工有限公司 | Preparation method of monocomponent moisturecured bonding agent for reflecting material |
| CN105295815A (en) * | 2015-11-11 | 2016-02-03 | 上海康达化工新材料股份有限公司 | Reactive polyurethane hot melt adhesive for reflective fabric and preparation method thereof |
| CN108165214A (en) * | 2018-01-03 | 2018-06-15 | 浙江恒劲树脂有限公司 | A kind of reflective preparation process for taking polyurethane resin composite glue |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110951419A (en) * | 2018-09-27 | 2020-04-03 | 江门市泰联新材料有限公司 | Hot melt adhesive |
| CN112297468A (en) * | 2020-10-13 | 2021-02-02 | 广东鸿驿聚氨酯科技有限公司 | Prepolymer and polyurethane seamless track for shot blasting machine and production process thereof |
| CN112297468B (en) * | 2020-10-13 | 2021-11-26 | 广东鸿驿聚氨酯科技有限公司 | Prepolymer and polyurethane seamless track for shot blasting machine and production process thereof |
| CN115181526A (en) * | 2021-08-30 | 2022-10-14 | 无锡博锦高分子研究发展有限公司 | Solvent-free washable reflective material adhesive and preparation method thereof |
| CN115181526B (en) * | 2021-08-30 | 2024-05-31 | 无锡博锦高分子研究发展有限公司 | Solvent-free washable reflective material adhesive and preparation method thereof |
| CN115584233A (en) * | 2022-02-22 | 2023-01-10 | 浙江星华反光材料有限公司 | Preparation process and application of high-toughness polyurethane adhesive |
| CN115584233B (en) * | 2022-02-22 | 2024-02-27 | 浙江星华反光材料有限公司 | Preparation process and application of high-toughness polyurethane adhesive |
| CN114957605A (en) * | 2022-07-04 | 2022-08-30 | 山东一诺威聚氨酯股份有限公司 | TPU (thermoplastic polyurethane) adhesive film material for traceless underwear and preparation method thereof |
| CN115820195A (en) * | 2022-08-15 | 2023-03-21 | 杭州星华反光材料股份有限公司 | Polyurethane glue for high-brightness reflective material and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111253899A (en) | Industrial water washing resistant bright silver reflective fabric adhesive and preparation method thereof | |
| CN103627362B (en) | A kind of reaction type polyurethane hot-melt adhesive and preparation method thereof | |
| CN103044665B (en) | Hydrolysis-resistant polyester polyol and preparation method thereof | |
| CN104804698A (en) | Bi-component composite adhesive for solar power back panel, and preparation method thereof | |
| CN106883810B (en) | High-peeling polyurethane adhesive | |
| CN110105530B (en) | Preparation method of UV (ultraviolet) moisture dual-curing resin | |
| CN105131896A (en) | Method for preparing polyurethane hot melt adhesive capable of achieving quick positioning | |
| CN104531038A (en) | Reaction type polyurethane hot-melt adhesive and preparation method thereof | |
| CN110776869B (en) | High-temperature-resistant high-strength polyurethane structural adhesive and preparation method thereof | |
| CN110372851B (en) | Synthesis method of flame-retardant polyol for wood glue with three functionality degrees and high cohesive energy | |
| CN109468114B (en) | High-performance polyurethane adhesive | |
| CN113637448A (en) | Single-component polyurethane corner-combining adhesive and preparation method thereof | |
| CN104817994B (en) | Fast-cured composite adhesive and preparation method thereof | |
| CN106367014A (en) | High-stretching-ratio-resisting adhesive for cable shielding film | |
| CN113292958A (en) | High-transparency environment-friendly silane modified polyether sealant and preparation method thereof | |
| CN112143435A (en) | Hot-melt reaction type polyurethane adhesive for compounding electronic nylon film | |
| CN115873225A (en) | Polyester epoxy diluent, epoxy adhesive and preparation method thereof | |
| CN104974338A (en) | Photocuring polyester polyol and application thereof in adhesives | |
| CN104650325B (en) | A kind of new polyester polyalcohol and preparation method thereof | |
| CN112980373B (en) | Isosorbide copolyester hot melt adhesive and preparation method thereof | |
| CN111978909B (en) | Reactive polyurethane hot melt adhesive for low-temperature coating and preparation method thereof | |
| CN110467898A (en) | A kind of PUR adhesive and preparation method thereof | |
| CN113698909A (en) | High-temperature-resistant polyurethane hot melt adhesive and preparation method thereof | |
| CN108728035B (en) | Self-catalytic polyurethane hot melt adhesive and preparation method thereof | |
| CN111909650A (en) | Moisture-curing polyurethane hot melt adhesive and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |