CN109401717B - A kind of modified polyurethane binder and preparation method thereof - Google Patents
A kind of modified polyurethane binder and preparation method thereof Download PDFInfo
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- CN109401717B CN109401717B CN201811251585.9A CN201811251585A CN109401717B CN 109401717 B CN109401717 B CN 109401717B CN 201811251585 A CN201811251585 A CN 201811251585A CN 109401717 B CN109401717 B CN 109401717B
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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
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
-
- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
-
- 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention provides a kind of modified polyurethane binder and preparation method thereof, the modified polyurethane binder includes component A and B component, in parts by mass, the component A includes following raw material components: 30-70 parts of polyether polyol, 0-5 parts of anti-settling agent, 1-10 parts of plasticizer A, 0-40 parts of filler A, 5-20 parts of isocyanates, 0.01-0.1 parts of catalyst, 0-0.5 parts of antioxidant, steady agent 0-0.5 parts of light；In parts by mass, the B component includes following raw material components: 10-30 parts of plasticizer B, 0-0.5 parts of emulsifier, 0-5 parts of water, 20-50 parts of filler B, 0.5-5 parts of performed polymer；Wherein the mass ratio of the component A and B component is 1:0.5-5.Binder of the invention can provide the sufficiently long rear viscous time, be conducive to the bonding construction of the sheet material and coiled material of large area.
Description
Technical field
The invention belongs to polyurethane adhesive technical field, it is related to a kind of modified polyurethane binder and preparation method thereof,
More particularly to the preparation method of modified polyurethane prepolymer and functional high thixotropic slurry.
Background technique
Polyurethane adhesive is an important component in the polyurethane resin currently grown rapidly, in many
Aspect is all widely used.However the isocyanates toxic monomers wherein to dissociate then use the polynary epoxy compound of terminal hydroxy group
Epoxy based polyurethanes are made in object and terminal isocyanate group base polyurethane prepolymer for use as, then are configured to polyurethane bonding with polyamine compounds
Agent.But this type polyurethane adhesive can not be applied well in some industries for needing live large-area construction, reason
It is that the reaction process of such polyurethane adhesive can not provide the sufficiently long rear viscous time, just viscous and surface drying time interval
It is short, it is unfavorable for the bonding construction of the sheet material and coiled material of large area.
Summary of the invention
In view of the problems of the existing technology, the object of the present invention is to provide a kind of modified polyurethane binders, just viscous
Fastly, thixotroping is high, and the viscous time is long afterwards, and bonding force is strong, superior performance；Invention also provides the modified polyurethane binders
Preparation method.
A kind of modified polyurethane binder, the modified polyurethane binder include component A and B component,
In parts by mass, the component A includes following raw material components:
In parts by mass, the B component includes following raw material components:
Wherein the mass ratio of the component A and B component is 1:0.5-5.
Further, the modified polyurethane binder includes component A and B component,
In parts by mass, the component A includes following raw material components:
In parts by mass, the B component includes following raw material components:
Wherein the mass ratio of the component A and B component is 1:1-3.
Further, the modified polyurethane binder includes component A and B component,
In parts by mass, the component A includes following raw material components:
In parts by mass, the B component includes following raw material components:
Wherein the mass ratio of the component A and B component is 1:2-2.5.
Further, the polyether polyol include poly- A1,15-25 parts of polyether polyol A2 of 15-25 parts of ethoxylated polyhydric alcohol and
5-15 parts of polyether polyol A3；The molecular weight of the polyether polyol A1 be 500-1500 (such as 800-1200, it is optional 1000),
Hydroxyl value 100-130mgKOH/g (optional 110-115mgKOH/g)；The molecular weight of the polyether polyol A2 is 3000-8000 (example
Such as 4000-6000, it is optional 5000), hydroxyl value 20-45mgKOH/g (optional 33-36mgKOH/g)；Point of the polyether polyol A3
Son amount be 1600-2800 (such as 1800-2200, it is optional 2000), hydroxyl value 48-70mgKOH/g (optional 54-56mgKOH/g).Institute
The preferred DL-1000D of polyether polyol A1, the polyether polyol A2 preferred DL-2000D of preferred EP-330N, polyether polyol A3 are stated,
It is produced by Shandong Lanxing Dongda Chemical Co., Ltd.
Further, the anti-settling agent is nanometer calcium carbonate and/or fumed silica.
It is further preferred that the granularity of the nanometer calcium carbonate is 0.01-0.1 μm, specific surface area 15-20m2/g；It is described
The specific surface area of fumed silica is 150-200m2/g。
Further, the plasticizer A is petroleum ester T-50 and/or dioctyl phthalate；Plasticizer B is petroleum ester
T-50 and/or chloro palm oil methyl ester.
Further, the catalyst is organotin catalysts, preferably dibutyltin dilaurate.
Optionally, the isocyanates is 10-15 parts；Optionally, the isocyanates is 15-20 parts.
Further, the isocyanates is 4,4- methyl diphenylene diisocyanate and/or 2,4- diphenyl methane two
Isocyanates, WANNATE MDI-50 (two isocyanide of diphenyl methane preferably produced by Wanhua Chemical Group Co., Ltd.
Acid esters -50).
Further, the antioxidant is 264, and the steady agent of light is UV-9.
Further, the emulsifier is alkyl phenol polyoxyethylene ether, preferred emulsifier OP-10.
Preferably, water used in the present invention is deionized water.
Further, the performed polymer is polyetheramine, and the amine value of the performed polymer is 150-200 mgKOH/g, preferably river
The CN03 of door long river chemical industry Industry Group Co., Ltd production.
Further, the filler A includes calcium carbonate, diatomite, nanometer calcium carbonate；The filler B includes calcium carbonate, silicon
Diatomaceous earth, nanometer calcium carbonate.
It is further preferred that the filler A is the calcium carbonate that granularity is 200-650 mesh (such as 400 mesh).
It is further preferred that filler B2, the filler B1 that the filler B includes B1 and 30-45 parts of filler of 1-3 parts are
Granularity is the diatomite of 200-650 mesh (such as 400 mesh), and the filler B2 is nanometer calcium carbonate.
A kind of preparation method of modified polyurethane binder, comprising the following steps:
(1) preparation of component A: polyether polyol, anti-settling agent, plasticizer A, filler A are added in reaction kettle and are stirred simultaneously
110-115 DEG C of heating, is dehydrated 1.5-2 hours, until cooling to 65-70 after moisture content≤200ppm at vacuum -0.095-0.1Mpa
DEG C, it is then added and isocyanates and keeps the temperature 1-3 hour (such as 2 hours), add catalyst and continue to keep the temperature 1-3 hours (such as 2
Hour), it then cools to 50-65 DEG C (such as 60 DEG C), antioxidant is added and the steady agent of light stirs evenly；5-25 points of cooling stirring
Clock, until the packaging that can discharge after 50 DEG C or less；
(2) preparation of B component: plasticizer B, emulsifier, water being added in container (such as dispersion cylinder) and are uniformly dispersed,
Middle emulsifier and water can be pre-mixed, high speed dispersion 5-25 minutes, be then added filler B, performed polymer be uniformly dispersed (or
Filler B1 is first added in cylinder and is uniformly dispersed by person, adds performed polymer and disperses 5-25 minutes, is eventually adding filler B2 progress
Height viscous dispersion 15-30 minutes)；The equipment used is high roll banding motivation, is dispersed to material in homogeneous without particle paste；
(3) component A is uniformly mixed with B component.
The construction usage method of product of the present invention is similar to existing technical products, and A, B component are mixed according to a certain percentage
Stirring is closed, directly has blade coating in substrate with band serrated knife, the thickness that the binder can be enabled to scrape 3-5mm due to having high thixotropic
Degree, it can be ensured that can have bonding coat between sheet material or coiled material and substrate, not occur hollowing phenomenon.
Compared with the existing technology, beneficial effects of the present invention:
(1) modified polyurethane binder of the invention preparation is simple, and raw material sources are wide；For modified polyetheramine performed polymer
Can in B component storage-stable, after being mixed into paste with nanometer calcium carbonate, not only can guarantee easy stirring, but also can guarantee high touching
Denaturation；
(2) during use, entire basis of reacting is still with one-component to modified polyurethane binder of the invention
Based on polyurethane, the polyureas reaction of gas is not released in the reaction of modifying moieties, can be provided and just be glued fastly in entire reaction process,
The high characteristic of intrinsic strength is formed, guarantee does not occur the phenomenon that coiled material or sheet material and substrate delamination hollowing；
(3) the main glue of modified polyurethane binder of the invention, i.e. monocomponent polyurethane accomplish no trip in formula design
Free isocyanate greatly extends the surface drying time in use process, while introducing enough water with emulsifier in B component
Part, so that the modified polyurethane binder surface drying time tends to close with the time is done solid work, when which provides longer rear viscous
Between, it can't influence to construct because of there is surface drying too early；
(4) modified polyurethane binder of the invention can embody the enough stickup time by features described above, i.e., just viscous
It can control 1-3 hours to surface drying (cannot bond), large-area construction when just eliminates the process that the whole audience presses, and does not have to
Worry, which is missed, pastes the time, or the delamination hollowing due to caused by coiled material or sheet material deformation alice；
(5) modified polyurethane binder of the invention is free of free isocyanate, is free of volatile solvent, can be used as environmental protection
Property binding material has passed through the most stringent of environmental protection standard Shanghai group environmental protection standard " T/310101002- of industry through inspection
C003-2016》。
Specific embodiment
In order to preferably explain the present invention, it is described further now in conjunction with following specific embodiments, but the present invention is unlimited
In specific embodiment.
Embodiment 1
A kind of modified polyurethane binder comprising component A and B component,
In parts by mass, the component A includes following raw material components:
The preparation of component A: by DL-1000D, EP-330N, DL-2000D for weighing up and fumed silica, plasticizer T-
50 and calcium carbonate (400 mesh) throw into reaction flask and stir and heat up 110-115 DEG C, vacuum -0.095-0.1Mpa be dehydrated 1.5-2
Hour, moisture content requirement≤200ppm cools to 65-70 DEG C, and isocyanates is added and keeps the temperature 2 hours, adds organotin catalysts
Continue heat preservation 2 hours, then cool to 60 DEG C, be added antioxidant -264 and light steady agent UV-9 cooling stirring 15 minutes, 50 DEG C with
Bottom discharge packaging.
In parts by mass, the B component includes following raw material components:
The preparation of B component: first the chloro palm oil methyl ester weighed up is thrown into dispersion cylinder, then the emulsification being pre-mixed
Agent OP-10 and aqueous solution are thrown into cylinder high speed and are dispersed 10 minutes, and then diatomite (400 mesh) is thrown into cylinder and is uniformly dispersed, then
Polyetheramine CN03 (amine value 150-200mgKOH/g) is put into and dispersed 10 minutes, finally nanometer calcium carbonate is put into and carries out height
Viscous dispersion 20 minutes.Device therefor is high roll banding motivation, is dispersed to material in homogeneous without particle paste.
Component A 100g, B component 250g are taken, is mixed evenly, 5mm high tooth blade coating simultaneously simulates stickup.
Embodiment 2
A kind of modified polyurethane binder comprising component A and B component,
In parts by mass, the component A includes following raw material components:
The preparation of component A: by DL-1000D, EP-330N, DL-2000D for weighing up and fumed silica, plasticizer T-
50 and calcium carbonate (400 mesh) throw into reaction flask and stir and heat up 110-115 DEG C, vacuum -0.095-0.1Mpa be dehydrated 1.5-2
Hour, moisture content requirement≤200ppm cools to 65-70 DEG C, and isocyanates is added and keeps the temperature 2 hours, adds organotin catalysts
Continue heat preservation 2 hours, then cool to 60 DEG C, be added antioxidant -264 and light steady agent UV-9 cooling stirring 15 minutes, 50 DEG C with
Bottom discharge packaging.
In parts by mass, the B component includes following raw material components:
The preparation of B component: first the chloro palm oil methyl ester weighed up is thrown into dispersion cylinder, then the emulsification being pre-mixed
Agent OP-10 and aqueous solution are thrown into cylinder high speed and are dispersed 10 minutes, and then diatomite (400 mesh) is thrown into cylinder and is uniformly dispersed, then
Polyetheramine CN03 is put into and dispersed 10 minutes, finally nanometer calcium carbonate is put into and carries out the viscous dispersion of height 20 minutes.Device therefor
For high roll banding motivation, material is dispersed in homogeneous without particle paste.
Component A 100g, B component 220g are taken, is mixed evenly, 5mm high tooth blade coating simultaneously simulates stickup.
Embodiment 3
A kind of modified polyurethane binder comprising component A and B component,
In parts by mass, the component A includes following raw material components:
The preparation of component A: by DL-1000D, EP-330N, DL-2000D for weighing up and fumed silica, plasticizer T-
50 and calcium carbonate (400 mesh) throw into reaction flask and stir and heat up 110-115 DEG C, vacuum -0.095-0.1Mpa be dehydrated 1.5-2
Hour, moisture content requirement≤200ppm cools to 65-70 DEG C, and isocyanates is added and keeps the temperature 2 hours, adds organotin catalysts
Continue heat preservation 2 hours, then cool to 60 DEG C, be added antioxidant -264 and light steady agent UV-9 cooling stirring 15 minutes, 50 DEG C with
Bottom discharge packaging.
In parts by mass, the B component includes following raw material components:
The preparation of B component: first the chloro palm oil methyl ester weighed up is thrown into dispersion cylinder, then the emulsification being pre-mixed
Agent OP-10 and aqueous solution are thrown into cylinder high speed and are dispersed 10 minutes, and then diatomite (400 mesh) is thrown into cylinder and is uniformly dispersed, then
Polyetheramine CN03 is put into and dispersed 10 minutes, finally nanometer calcium carbonate is put into and carries out the viscous dispersion of height 20 minutes.Device therefor
For high roll banding motivation, material is dispersed in homogeneous without particle paste.
Component A 100g, B component 200g are taken, is mixed evenly, 5mm high tooth blade coating simultaneously simulates stickup.
Modified polyurethane binder of the invention has passed through the most stringent of environmental protection standard Shanghai group environmental protection of industry through inspection
Standard " T/310101002-C003-2016 ".Testing result be listed in table 1 (Shanghai Jianke Inspection Co., Ltd, report number:
PD278-180086)。
Table 1: the inspection examining report of modified polyurethane binder of the invention.
As shown in Table 1, every Testing index of modified polyurethane binder of the invention meets Shanghai group environmental protection mark
It is quasi-.
Comparative example 1 is the similar binder of the prior art, two-component epoxies binder.
Comparative example 2 is same as Example 1, the difference is that DL-1000D of the polyether polyol only with 50 parts.
Comparative example 3 is same as Example 1, the difference is that being added without organotin catalysts.
Comparative example 4 is same as Example 1, the difference is that the amine value of the polyetheramine used is 220-500mgKOH/g.
Table 2: performance detection.
As can be seen from Table 2, modified polyurethane binder of the invention binder (comparative example 1 similar for the prior art
(two-component epoxies binder)), it can be first viscous time speed-raising degree to 30min, and when surface drying under same execution conditions
Between postpone so that thereafter glue the time elongate, be more suitable for live large-area construction, it is easier to grasp construction paste the time, it is not easy to
There is hollowing alice and other issues.
Above is only a specific embodiment of the present invention, it is not intended to limit the scope of the invention, all utilizations
The equivalent transformation that the present invention makees, is applied directly or indirectly in other relevant technical fields, similarly includes of the invention
Among scope of patent protection.
Claims (8)
1. a kind of modified polyurethane binder, which is characterized in that the modified polyurethane binder includes component A and B component, is pressed
Mass parts meter, the component A include following raw material components:
In parts by mass, the B component includes following raw material components:
Wherein the mass ratio of the component A and B component is 1:0.5-5；
The polyether polyol includes 15-25 parts of polyether polyol A1,15-25 part A2 and 5-15 parts of polyether polyols of polyether polyol
Alcohol A3；The molecular weight of the polyether polyol A1 is 500-1500, hydroxyl value 100-130mgKOH/g；The polyether polyol A2's
Molecular weight is 3000-8000, hydroxyl value 20-45mgKOH/g；The molecular weight of the polyether polyol A3 is 1600-2800, hydroxyl value
48-70mgKOH/g；
The catalyst is organotin catalysts；The performed polymer is polyetheramine, and the amine value of the performed polymer is 150-
200mgKOH/g。
2. modified polyurethane binder according to claim 1, which is characterized in that the modified polyurethane binder includes
Component A and B component,
In parts by mass, the component A includes following raw material components:
In parts by mass, the B component includes following raw material components:
Wherein the mass ratio of the component A and B component is 1:1-3.
3. modified polyurethane binder according to claim 1, which is characterized in that the modified polyurethane binder includes
Component A and B component,
In parts by mass, the component A includes following raw material components:
In parts by mass, the B component includes following raw material components:
Wherein the mass ratio of the component A and B component is 1:2-2.5.
4. modified polyurethane binder according to any one of claim 1-3, which is characterized in that the anti-settling agent is to receive
Rice calcium carbonate and/or fumed silica；The granularity of the nanometer calcium carbonate is 0.01-0.1 μm, specific surface area 15-20m2/g；
The specific surface area of the fumed silica is 150-200m2/g。
5. modified polyurethane binder according to any one of claim 1-3, which is characterized in that the plasticizer A is
Petroleum ester T-50 and/or dioctyl phthalate；Plasticizer B is petroleum ester T-50 and/or chloro palm oil methyl ester.
6. modified polyurethane binder according to any one of claim 1-3, which is characterized in that the isocyanates is
4,4 '-methyl diphenylene diisocyanates and/or 2,4- methyl diphenylene diisocyanate；The emulsifier is alkyl phenol polyoxy
Vinethene.
7. modified polyurethane binder according to any one of claim 1-3, which is characterized in that the filler A includes
Calcium carbonate, diatomite, nanometer calcium carbonate；The filler B includes calcium carbonate, diatomite, nanometer calcium carbonate.
8. modified polyurethane binder according to claim 7, which is characterized in that it is 200-650 that the filler A, which is granularity,
Purpose calcium carbonate；The filler B includes the filler B2 of B1 and 30-45 parts of filler of 1-3 parts, and it is 200- that the filler B1, which is granularity,
The diatomite of 650 mesh, the filler B2 are nanometer calcium carbonate.
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| CN201811251585.9A CN109401717B (en) | 2018-10-25 | 2018-10-25 | A kind of modified polyurethane binder and preparation method thereof |
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| GB0505587D0 (en) * | 2005-03-17 | 2005-04-27 | Dsm Ip Assets Bv | Aqueous polyurethane compositions |
| DE102007062316A1 (en) * | 2007-12-21 | 2009-06-25 | Evonik Degussa Gmbh | Reactive isocyanate compositions |
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Denomination of invention: A modified polyurethane adhesive and its preparation method Effective date of registration: 20230911 Granted publication date: 20191018 Pledgee: Jiangmen Rural Commercial Bank Co.,Ltd. Gujing sub branch Pledgor: JIANGMEN CHANGHE CHEMICAL INDUSTRY GROUP Co.,Ltd. Registration number: Y2023980056154 |
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