CN104559899A - Polyaspartate polyurea adhesive and preparation method thereof - Google Patents
Polyaspartate polyurea adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyaspartate polyurea adhesive and a preparation method thereof. The polyaspartate polyurea adhesive comprises a component A and a component B spaced from each other before being used, wherein the component A and the component B are mixed at a weight ratio of 4 to (1-1.05) when being used; the component A comprises the following components in parts by weight: 4.0-5.0 parts of polyaspartate polyurea, 4.0-4.50 parts of fillers, 0.005-0.01 parts of a defoamer and 0.005-0.01 parts of a leveling agent; the component B is hexamethylene diisocyanate trimer. According to the polyaspartate polyurea adhesive, the component A and the component B are mixed, so that the bonding strength in a bonding process is high and especially the bonding strength between the adhesive and a cement matrix is high; moreover, the adhesive has excellent performances of chemical corrosion resistance, water resistance, weather resistance, temperature resistance, low VOC (volatile organic compounds), environmental protection and the like.
Description
Technical field
The present invention relates to sizing agent technical field, particularly a kind of polyaspartate polyurea sizing agent and preparation method thereof.
Background technology
Glued joint (bonding, bonding, cementing, gluing) and refer to the technology that homogeneity or heterogeneous body surface sizing agent link together, there is stress distribution continuous, lightweight, or sealing, the features such as most technological temperature is low.Glued joint the connection being specially adapted to unlike material, different thickness, ultra-thin specification and complex component.Show from cementitious system breaking test, also show four kinds of different situations during glue-joint failure: 1. interfacial failure: adhesive layer all separates with sticky surface (the complete disengaging in gluing interface); 2. Cohesive failure: destroy and occur in sizing agent or clung body itself, and not between gluing interface; 3. mixing destroy: adherend and adhesive layer itself have partial destruction or both in only have one.These destroy and illustrate that bonding strength is not only relevant with by the intermolecular forces of stick and adherend, and the reactive force also and between the molecule of polymkeric substance sizing is relevant.
The sorting technique of sizing agent is a lot, can be divided into heat curing-type, hot-melting type, room temperature curing type, pressure sensitive etc. by application method.Structure-type, non-configuration or special gelatin is divided into by application.Connect form and can be divided into water-soluble, water-latex type, solvent-borne type and various solid-state versions etc.Tradition sizing agent production cost is high, and result of use is bad.Along with the high speed development of Chinese national economy and improving constantly of living standards of the people.The use range of sizing agent is more and more wider, requires also more and more higher to its intensity or other performances etc.Concrete, as the lifting along with architect's design concept, buildings is more and more high-grade, multifunctional direction development, this sizing agent is more and more widely used at building field, except having except requirement to sizing agent intensity, also develops its water tolerance, resistance to chemical attack, weathering resistance, temperature tolerance, the performance requriementss such as low VOC environmental protection are also more and more higher.
And due to specific industry requirements such as such as buildings, the intensity of existing sizing agent intensity particularly and between cement matrix, resistance to chemical corrosion and the performance such as weathering resistance and environmental protection are undesirable, therefore, the sizing agent how developing particularly suitable and building trade is very necessary.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of polyaspartate polyurea sizing agent and preparation method thereof is provided, low to overcome existing sizing agent cohesive strength, the technical problem that chemical resistance and weathering resistance are not strong.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of polyaspartate polyurea sizing agent, comprise A spaced before use, B component, the weight ratio of described A, B is 4:(1-1.05); Wherein,
Described component A comprises the composition of following weight part:
Polyaspartate polyurea 4.0-5.0 part
Filler 4.0-4.5 part
Defoamer 0.005-0.01 part
Flow agent 0.005-0.01 part;
Described B component is: hexamethylene diisocyanate trimer.
And a kind of preparation method of polyaspartate polyurea sizing agent, comprises the steps:
The step that the preparation method of component A comprises: after obtaining each raw material respectively according to the composition in the component A of the invention described above polyaspartate polyurea sizing agent and content, each component is carried out mixing treatment;
Obtain B component hexamethylene diisocyanate trimer;
By the A of preparation, B component separately packaging.
Polyaspartate polyurea sizing agent of the present invention by A, that B component is blended in cohesive strength in bonding process is high, the cohesive strength particularly and between cement matrix is high, and has excellent resistance to chemical attack, water tolerance, resistance to chemical attack, weathering resistance, temperature tolerance, the performances such as low VOC environmental protection.Above-mentioned polyaspartate polyurea sizing agent preparation method only needs each component to be added by step according to component A formula respectively, through mixing treatment, each component is fully mixed, also without the need to special equipment, therefore, the method technique is simple, be applicable to suitability for industrialized production, saved energy consumption, reduced cost.And the polyaspartate polyurea sizing agent stable performance of preparation, it is low containing VOC composition, its production safety environmental protection.
Accompanying drawing explanation
Fig. 1 is method flow diagram prepared by the embodiment of the present invention 1 polyaspartate polyurea sizing agent.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of cohesive strength high, the polyaspartate polyurea sizing agent that weather-proof resistance to chemical corrosion is good.This polyaspartate polyurea sizing agent comprises A, B component hereinafter described.In this polyaspartate polyurea sizing agent product, A, B component are spaced, realize spaced as adopted the mode of separately packaging.So in the product of this polyaspartate polyurea sizing agent, A, B component can carry out separately packaging according to arbitrary ratio, only need A, B component to be carried out mixing according to certain ratio when in use.In order to ensure the cohesive strength of embodiment of the present invention polyaspartate polyurea sizing agent, in one embodiment, be 4:(1-1.05 by described A, B according to weight ratio during use) mix.Therefore, in order to the convenience used, in one embodiment, in the packing of product before use, be 4:(1-1.05 by described A, B component according to weight ratio) carry out separately packaging, in use, without the need to measuring, directly described A, B component being carried out mixing and can use.
Wherein, above-mentioned component A comprises the composition of following weight part:
Polyaspartate polyurea 4.0-5.0 part
Filler 4.0-4.5 part
Defoamer 0.005-0.01 part
Flow agent 0.005-0.01 part.
Particularly, this polyaspartate polyurea is as the matrix component of component A, and it is to the cohesive strength of embodiment of the present invention polyaspartate polyurea sizing agent, corrosion-resistant, water-fast, and the performances such as heatproof have important decisive role impact.
In one embodiment, ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane (DMDC) are carried out reaction and prepare by this polyaspartate polyurea at 60-80 DEG C.In certain embodiments, in the system that ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane react, the weight ratio of this ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane is 1.5:(2.1-2.7).In one embodiment, the weight ratio of this ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane is 1.73:2.71.The polyaspartate polyurea prepared by the method is to the cohesive strength of polyaspartate polyurea sizing agent of the present invention, and corrosion-resistant, water-fast, the performances such as heatproof have castering action.
In another specific embodiment, the content of this polyaspartate polyurea in component A is the weight parts such as 4.4 parts, 4.5 parts, 5.0 parts.
Above-mentioned filler is filled sizing agent of the present invention, and strengthen hardness, therefore, in one embodiment, one or more the mixture in kaolin, water-ground limestone, the above fine sand of 200 order etc. selected by this filler.In certain embodiments, this filler is the mixture of kaolin and water-ground limestone, and the weight ratio of kaolin and water-ground limestone is 1:(0.8-1.2).In one embodiment, this filler is the mixture of kaolin and coarse whiting, and the weight ratio of kaolin and coarse whiting is 1:1.
In another specific embodiment, the content of this filler in component A is the weight parts such as 4 parts, 4.5 parts.
In one embodiment, bubble polysiloxane defoamer selected brokenly by above-mentioned defoamer.In certain embodiments, the content of this defoamer in component A can be the weight part such as 0.005 part, 0.01 part.In one embodiment, above-mentioned flow agent selects polyether modified siloxane class flow agent.In certain embodiments, the content of this flow agent in component A can be the weight part such as 0.005 part, 0.01 part.
Therefore, in one embodiment, above-mentioned component A can also be the composition of following parts by weight:
Polyaspartate polyurea 4.4 parts
Filler 4 parts
Defoamer 0.005 part
Flow agent 0.005 part.
The controlling and adjustment of the poly-component A content of preferred proportion component should be contained, make polyaspartate polyurea sizing agent have more excellent cohesive strength, resistance to chemical attack and water-repellancy and weather resistance.When component A comprises the composition of this concrete content, in use, described A, B component are that 4:1 mixes according to weight ratio, in packaging are so, and A, B component can be that 4:1 carries out separately packaging according to weight ratio.
Above-mentioned B component is hexamethylene diisocyanate trimer.
From the above mentioned, in the various embodiments described above polyaspartate polyurea sizing agent by A, that B component is blended in cohesive strength in bonding process is high, cohesive strength particularly and between cement matrix is high, and there is excellent resistance to chemical attack, water tolerance, resistance to chemical attack, weathering resistance, temperature tolerance, the performances such as low VOC environmental protection.In addition, by the control to constituent species and content, the cohesive strength that can promote polyaspartate polyurea sizing agent is further high, and has excellent resistance to chemical attack, water tolerance, resistance to chemical attack, weathering resistance, temperature tolerance, the performances such as low VOC environmental protection.
Correspondingly, the embodiment of the present invention additionally provides a kind of preparation method of above-mentioned polyaspartate polyurea sizing agent.This preparation method comprises the steps:
The step that the preparation method of step S01. component A comprises: after obtaining each raw material respectively according to the composition in the component A of polyaspartate polyurea sizing agent mentioned above and content, each component is carried out mixing treatment;
Step S02. obtains B component hexamethylene diisocyanate trimer;
Step S03. is by the A of preparation, B component separately packaging.
Particularly, in above-mentioned steps S01, each component of component A as described above, in order to save length, does not repeat them here.
Wherein, polyaspartate polyurea can prepare acquisition according to polyaspartate polyurea preparation method mentioned above.In one embodiment, when adopting that method prepares polyaspartate polyurea above, be add in reactor to react by ethyl maleate and N-hydroxyalkyl quaternary ammonium hydroxide.Owing to being employing ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane reactant, therefore, without the need to adding reaction solvent in addition.
In this step S01, the composition that component A is carried out contained by mixing treatment component A is mixed, therefore in order to realize mixing of each composition.
In one embodiment, if this polyaspartate polyurea be according to above by ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane carries out reaction when preparing, all the other of component A directly can be accessed ethyl maleate and 3, mixing treatment is carried out in reaction solution after the reaction of 3-dimethyl-4,4-diamino-dicyclohexyl methane terminates.
In one embodiment, the method obtaining B component hexamethylene diisocyanate trimer in above-mentioned steps S02 is as follows:
Hexamethylene diisocyanate (HDI) and catalyzer are reacted at 60-70 DEG C, produces hexamethylene diisocyanate trimer.
In one embodiment, the weight ratio of this hexamethylene diisocyanate and N-hydroxyalkyl quaternary ammonium hydroxide is 1:(0.03-0.05).In one embodiment, catalyzer is at least one in N-hydroxyalkyl quaternary ammonium hydroxide, tributyltin oxide, tetrabutyl chromic oxide etc.Be reaction owing to being hexamethylene diisocyanate, therefore, without the need to adding reaction solvent in addition.
In one embodiment, judging that hexamethylene diisocyanate and N-hydroxyalkyl quaternary ammonium hydroxide react the standard terminated is that the NCO content's index in reaction product is qualified.In one embodiment, the standard that this NCO content's index is qualified is NCO content is (20%-21%).After hexamethylene diisocyanate and N-hydroxyalkyl quaternary ammonium hydroxide react and terminate, distillation can obtain hexamethylene diisocyanate trimer.
In addition, there is no sequencing when above-mentioned steps S01 and step S02 implements, can carry out flexibly according to actual production.
In above-mentioned steps S03, when A, B component are separately packed, as above-mentioned above, the amount of A, B component does not specially require, only need be spaced by A, B component.In other words in the product of this polyaspartate polyurea sizing agent, A, B component can carry out separately packaging according to arbitrary ratio, only need A, B component to be carried out mixing according to certain ratio when in use.In order to ensure the cohesive strength of embodiment of the present invention polyaspartate polyurea sizing agent, in one embodiment, be 4:(1-1.05 by described A, B according to weight ratio during use) mix.Therefore, in order to the convenience used, in one embodiment, in the packing of product before use, be 4:(1-1.05 by described A, B component according to weight ratio) carry out separately packaging, in use, without the need to measuring, directly described A, B component being carried out mixing and can use.
Above-mentioned polyaspartate polyurea sizing agent preparation method only need prepare A, B component respectively, then A, B are divided to open and pack, without complicated procedures of forming, also without the need to special equipment, make the method technique simple, be applicable to suitability for industrialized production, saved energy consumption, reduce cost, and the polyaspartate polyurea sizing agent stable performance of preparation.
Now with concrete polyaspartate polyurea sizing agent formula and be prepared as example, the present invention is further elaborated.Wherein, the kind of filler hereinafter and defoamer, flow agent all as indicated above.
embodiment 1
A kind of polyaspartate polyurea sizing agent and preparation method thereof.This polyaspartate polyurea sizing agent comprises A spaced before use, B component, during use described A, B component according to weight ratio for 4:1 mixes; Wherein,
Described component A comprises the composition of following weight part:
Polyaspartate polyurea 4.4 parts
Kaolin 2 parts
Water-ground limestone 2 parts
Defoamer 0.005 part
Flow agent 0.005 part;
Described B component is: hexamethylene diisocyanate trimer.
As shown in Figure 1, it comprises following steps in its preparation method technical process:
S11. ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane that weight ratio is 1.73:2.71 is added in a kettle., be warming up to 60-80 DEG C, stir lower reaction 72 hours, be cooled to room temperature, obtain the reaction solution containing polyaspartate polyurea;
S12. in the reaction solution of step S11, add kaolin, coarse whiting and defoamer, flow agent, dispersed with stirring 25 minutes, discharging, be packaged to be polyaspartate polyurea sizing agent component A;
S13. hexamethylene diisocyanate and N-hydroxyalkyl quaternary ammonium hydroxide are reacted at 60-70 DEG C, until stopped reaction when the NCO content's index in reaction soln reaches 20%, carry out packing pack dress after distillation process and obtain polyaspartate polyurea sizing agent B component.
embodiment 2
A kind of polyaspartate polyurea sizing agent and preparation method thereof.This polyaspartate polyurea sizing agent comprises A spaced before use, B component, during use described A, B component according to weight ratio for 4:1 mixes; Wherein,
Described component A comprises the composition of following weight part:
Polyaspartate polyurea 4.6 parts
Kaolin 2 parts
200 order fine sands 2.2 parts
Defoamer 0.005 part
Flow agent 0.005 part;
Described B component is: hexamethylene diisocyanate trimer.
As shown in Figure 1, it comprises following steps in its preparation method technical process:
S21. ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane that weight ratio is 1.80:2.80 is added in a kettle., be warming up to 60-80 DEG C, stir lower reaction 72 hours, be cooled to room temperature, obtain the reaction solution containing polyaspartate polyurea;
S22. in the reaction solution of step S21, add kaolin, 200 order fine sands and defoamer, flow agent, dispersed with stirring 25 minutes, discharging, be packaged to be polyaspartate polyurea sizing agent component A;
S23. hexamethylene diisocyanate and tetrabutyl chromic oxide are reacted at 60-70 DEG C, until stopped reaction when the NCO content's index in reaction soln reaches 20%, carry out packing pack dress after distillation process and obtain polyaspartate polyurea sizing agent B component.
embodiment 3
A kind of polyaspartate polyurea sizing agent and preparation method thereof.This polyaspartate polyurea sizing agent comprises A spaced before use, B component, during use described A, B component according to weight ratio for 4:1 mixes; Wherein,
Described component A comprises the composition of following weight part:
Polyaspartate polyurea 5 parts
Water-ground limestone 2.2 parts
200 order fine sands 2.3 parts
Defoamer 0.01 part
Flow agent 0.01 part;
Described B component is: hexamethylene diisocyanate trimer.
As shown in Figure 1, it comprises following steps in its preparation method technical process:
S31. ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane that weight ratio is 1.95:3.05 is added in a kettle., be warming up to 60-80 DEG C, stir lower reaction 72 hours, be cooled to room temperature, obtain the reaction solution containing polyaspartate polyurea;
S32. in the reaction solution of step S31, add water-ground limestone, 200 order fine sands and defoamer, flow agent, dispersed with stirring 25 minutes, discharging, be packaged to be polyaspartate polyurea sizing agent component A;
S33. hexamethylene diisocyanate and tetrabutyl chromic oxide are reacted at 60-70 DEG C, until stopped reaction when the NCO content's index in reaction soln reaches 20%, carry out packing pack dress after distillation process and obtain polyaspartate polyurea sizing agent B component.
comparative example
Existing market sizing agent
performance test
The existing market sizing agent provided in the polyaspartate polyurea sizing agent provided by above-described embodiment 1-3 and comparative example carries out the correlated performance test in following table 1 respectively, and test result is as following table 1.
table 1
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a polyaspartate polyurea sizing agent, comprises A spaced before use, B component, and during use, described A, B component are 4:(1-1.05 according to weight ratio) mix; Wherein, described component A comprises the composition of following weight part: polyaspartate polyurea 4.0-5.0 part
Filler 4.0-4.5 part
Defoamer 0.005-0.01 part
Flow agent 0.005-0.01 part;
Described B component is: hexamethylene diisocyanate trimer.
2. polyaspartate polyurea sizing agent according to claim 1, is characterized in that: in described component A:
Polyaspartate polyurea 4.4 parts
Filler 4 parts
Defoamer 0.005 part
Flow agent 0.005 part.
3. polyaspartate polyurea sizing agent according to claim 2, is characterized in that: during use described A, B component according to weight ratio for 4:1 mixes.
4. the polyaspartate polyurea sizing agent according to any one of claim 1-3, it is characterized in that: described polyaspartate polyurea is by ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane carries out reaction and prepares at 60-80 DEG C.
5. polyaspartate polyurea sizing agent according to claim 4, is characterized in that: the weight ratio of described ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane is 1.5:(2.1-2.7).
6. polyaspartate polyurea sizing agent according to claim 4, is characterized in that: the weight ratio of described ethyl maleate and 3,3-dimethyl-4,4-diamino-dicyclohexyl methane is 1.73:2.71.
7. according to claim 1-3,5, polyaspartate polyurea sizing agent described in 6 any one, it is characterized in that: one or more the mixture in kaolin, coarse whiting, the above fine sand of 200 order selected by described filler.
8. according to claim 1-3,5,6 arbitrary described polyaspartate polyurea sizing agents, it is characterized in that: described filler is the mixture of kaolin and coarse whiting, and the weight ratio of kaolin and water-ground limestone is 1:(0.8-1.2).
9. polyaspartate polyurea sizing agent according to claim 3, is characterized in that: bubble polysiloxane defoamer selected brokenly by described defoamer; Or/and described flow agent selects polyether modified siloxane class flow agent.
10. a preparation method for polyaspartate polyurea sizing agent, comprises the steps:
The step that the preparation method of component A comprises: after obtaining each raw material respectively according to the composition in the component A of the polyaspartate polyurea sizing agent described in any one of claim 1-9 and content, each component is carried out mixing treatment;
Obtain B component hexamethylene diisocyanate trimer; By the A of preparation, B component separately packaging.
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| CN110845685A (en) * | 2019-12-12 | 2020-02-28 | 中国科学院长春应用化学研究所 | Polyaspartic acid ester and polyurea-based repairing material for repairing polyurethane foam of automobile instrument panel, and preparation method and repairing method thereof |
| CN111303368A (en) * | 2020-04-22 | 2020-06-19 | 深圳飞扬骏研新材料股份有限公司 | Water-based polyaspartic acid ester resin and preparation method thereof |
| CN111303368B (en) * | 2020-04-22 | 2021-09-17 | 深圳飞扬骏研新材料股份有限公司 | Water-based polyaspartic acid ester resin and preparation method thereof |
| CN111410919A (en) * | 2020-05-12 | 2020-07-14 | 江西蓝海芯科技集团有限公司 | Protection film convenient to recycle |
| CN115785877A (en) * | 2022-12-15 | 2023-03-14 | 厦门昕钢防腐工程科技有限公司 | Strong-corrosion-resistance ultralow-temperature bonding adhesive and preparation method and application thereof |
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Application publication date: 20150429 |