A kind of THIXCIN intercalation polynite thixotropic agent and preparation method thereof
Technical field
The present invention relates to the thixotropic agent technical field, particularly relate to a kind of THIXCIN intercalation polynite thixotropic agent and preparation method thereof.
Background technology
Polyurethane sealant is because characteristic such as its adhesiveproperties is strong, mechanics superior and acid and alkali-resistance, organic solvent-resistant are good is widely used in fields such as automobile assembling, building sealing.
Yet, when one-component polyurethane sealant is applied to the facade filleting of buildings, because own wt causes the anti-sag performance poor.Therefore, in order to improve the anti-sag performance of one-component polyurethane sealant, need in one-component polyurethane sealant, to add thixotropic agent.
Thixotropic agent is called anti-sagging agent again, is a kind of auxiliary agent that can make colloid produce " thixotroping phenomenon ".When the time spent of doing that colloid receives shearing force, denseness descends, and shearing force is big more, and the denseness decline scope is also big more; Remove back (when being interrupted as stirring or shearing) when shearing force, denseness slowly returns to not runny originally state again.The effect of thixotropic agent is to prevent that colloid from trickling on inclined-plane of constructing or vertical surface, avoids colloidal content that the uneven phenomenon of levels is arranged, thereby guarantees the quality of product; And have than low-viscosity under the high shear rate when construction, help colloid to flow and be easy to construct; Have than high viscosity under the low shear rate after before construction, reaching, can prevent pigment sedimentation and wet film sagging.
In the prior art, thixotropic agent commonly used in one-component polyurethane sealant mainly includes aerosil, organobentonite, hydrogenated castor wet goods.Aerosil, because specific surface area is high, tap density is light, thus need special devices to disperse, and because its particle surface is prone to suction, be difficult in mono-component polyurethane, use.Organic expander profit soil, though have good anti-sag performance, add a certain amount of organobentonite after, be prone to cause the increase of sealer modulus, be difficult to polyurethane sealant is prepared into the product of low modulus, make it not used widely thus.THIXCIN, though have good anti-sag performance, because its molecular structure is a polyhydroxy substance; When it is applied to one-component polyurethane sealant, is prone to form gel, thereby influences the outward appearance and the memory property of product; Under hot conditions, its thixotropic property obviously reduces simultaneously.
Therefore, to deficiency of the prior art, need badly:
(1) a kind of good environmental adaptability is provided, can under different temperature, all has good anti-sag performance, and with the consistency of polyurethane sealant better, be prone to disperse, make the sealer modulus less THIXCIN intercalation polynite thixotropic agent that raises.
(2) a kind of preparation method of THIXCIN intercalation polynite thixotropic agent is provided; It is strong to adopt this preparation method to prepare environmental compatibility; Can under differing temps, have good anti-sag performance; And disperse the THIXCIN intercalation polynite thixotropic agent that the rising of sealer modulus is less with the consistency of polyurethane sealant is better, easy.
Summary of the invention
One of the object of the invention is to avoid weak point of the prior art and a kind of good environmental adaptability is provided; Can under different temperature, all have good anti-sag performance; And with the consistency of polyurethane sealant better, be prone to disperse, make the sealer modulus less THIXCIN intercalation polynite thixotropic agent that raises.
Two of the object of the invention is to avoid weak point of the prior art and preparation method that a kind of THIXCIN intercalation polynite thixotropic agent is provided; It is strong to adopt this preparation method to prepare environmental compatibility; Can under differing temps, have good anti-sag performance; And with the consistency of polyurethane sealant better, be prone to disperse, make the sealer modulus less THIXCIN intercalation polynite thixotropic agent that raises.
The object of the invention is realized through following technical scheme:
A kind of THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
1~20 part of organo montmorillonite
1~30 part of THIXCIN
20~1000 parts of dry toluenes
3~10 parts of active hydrogen scavenging agents.
Preferably, described THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
1~10 part of organo montmorillonite
1~20 part of THIXCIN
20~600 parts of dry toluenes
3~6 parts of active hydrogen scavenging agents.
More preferably, described THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
1 part of organo montmorillonite
5 parts of THIXCINs
20 parts of dry toluenes
3 parts of active hydrogen scavenging agents.
Preferably, described THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
10~20 parts of organo montmorillonites
20~30 parts of THIXCINs
600 ~ 1000 parts of dry toluenes
6~10 parts of active hydrogen scavenging agents.
More preferably, described THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
20 parts of organo montmorillonites
25 parts of THIXCINs
1000 parts of dry toluenes
10 parts of active hydrogen scavenging agents.
Wherein, said organo montmorillonite is the ammonium polynite.
Wherein, the carbon content number of organic ammonium is 5 ~ 20 in the said ammonium polynite.
Wherein, said active hydrogen scavenging agent is the compsn of organic acid anhydride and quicklime, and contains a kind of in the simple function group isocyanic ester or two kinds.
The present invention also provides a kind of preparation method of THIXCIN intercalation polynite thixotropic agent, may further comprise the steps:
Step 1 is prepared raw material by above-mentioned weight part;
Step 2 with raw material organo montmorillonite, THIXCIN and dry toluene, is added in the duplicate rows star reaction kettle that the high speed dispersion dish is housed, and is warming up to 80 ~ 120 ℃, refluxing and stirring 2 ~ 3h;
Step 3, decompression vacuum pumping is removed toluene;
Step 4, temperature remain on 110 ~ 120 ℃, and high temperature vacuumizes 3h and removes steam;
Step 5 is cooled to 40 ~ 60 ℃, adds the active hydrogen scavenging agent, continues to stir 0.5h, goes out the still sealing, promptly gets THIXCIN intercalation polynite thixotropic agent.
Wherein, in the said step 2,, be added in the duplicate rows star reaction kettle that the high speed dispersion dish is housed, be warming up to 100 ~ 120 ℃ raw material organo montmorillonite, THIXCIN and dry toluene.
Beneficial effect of the present invention: THIXCIN intercalation polynite thixotropic agent of the present invention comprises the raw material of following weight part: 1~20 part of organo montmorillonite, 1~30 part of THIXCIN, 20 ~ 1000 parts of dry toluenes, 3~10 parts of active hydrogen scavenging agents.The preparation method of THIXCIN intercalation polynite thixotropic agent of the present invention may further comprise the steps: step 1, prepare raw material by above-mentioned weight part; Step 2 with raw material organo montmorillonite, THIXCIN and dry toluene, is added in the duplicate rows star reaction kettle that the high speed dispersion dish is housed, and is warming up to 80 ~ 120 ℃, refluxing and stirring 2 ~ 3h; Step 3, decompression vacuum pumping is removed toluene; Step 4, temperature remain on 110 ~ 120 ℃, and high temperature vacuumizes 3h and removes steam; Step 5 is cooled to 40 ~ 60 ℃, adds the active hydrogen scavenging agent, continues to stir 0.5h, goes out the still sealing, promptly gets THIXCIN intercalation polynite thixotropic agent.Compared with prior art; Composition and the formed THIXCIN intercalation of proportioning polynite thixotropic agent according to 1~20 part of organo montmorillonite, 1~30 part of THIXCIN, 20 ~ 1000 parts of dry toluenes, 3~10 parts of active hydrogen scavenging agents; Have be prone to disperse, characteristics that thixotropic property is good, and environmental compatibility is strong, can consistency preferably be arranged with polyurethane sealant; Under differing temps, all have good anti-sag performance, and the sealer modulus raises less.
Embodiment
In conjunction with following examples the present invention is further described:
Need to prove that the sealing glue solidifying condition is 23 ℃ in following examples, relative humidity 50 ﹪ held 3 days are then 50 ℃ of held 5 days.Tensile modulus is pressed method mensuration, the droop test of GB/T13477.8-2002 Test method for building sealants the 8th part stretching cementability and is pressed the extrudability method test of GB/T13477.3-2002 Test method for building sealants the 3rd part use standard utensil mensuration sealing material.
Embodiment 1
A kind of THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
20 parts of ammonium polynites
25 parts of THIXCINs
1000 parts of dry toluenes
To 10 parts of Methyl benzenesulfonyl isocyanates.
Wherein, the carbon content number of organic ammonium is 5 in the ammonium polynite.
Embodiment 2
A kind of THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
1 part of ammonium polynite
5 parts of THIXCINs
20 parts of dry toluenes
3 parts of the compsns of Tetra hydro Phthalic anhydride and quicklime.
Wherein, the carbon content number of organic ammonium is 8 in the ammonium polynite.
Wherein, Tetra hydro Phthalic anhydride and quicklime can mix by arbitrary proportion.
Embodiment 3
A kind of THIXCIN intercalation polynite thixotropic agent comprises the raw material of following weight part:
10 parts of ammonium polynites
18 parts of THIXCINs
200 parts of dry toluenes
To 10 parts of Methyl benzenesulfonyl isocyanates.
Wherein, the carbon content number of organic ammonium is 15 in the ammonium polynite.
Embodiment 4
A kind of preparation method of THIXCIN intercalation polynite thixotropic agent may further comprise the steps:
Step 1, the weight part of pressing among the embodiment 1 is formed the preparation raw material;
Step 2 with 1000 parts of 20 parts of raw material ammonium polynites, 25 parts of THIXCINs and dry toluenes, is added in the duplicate rows star reaction kettle that the high speed dispersion dish is housed, and is warming up to 120 ℃, refluxing and stirring 3h;
Step 3, decompression vacuum pumping is removed toluene;
Step 4, temperature remain on 120 ℃, and high temperature vacuumizes 3h and removes steam;
Step 5 is cooled to 60 ℃, adds 10 parts of Methyl benzenesulfonyl isocyanates, continues to stir 0.5h, goes out the still sealing, promptly gets THIXCIN intercalation polynite thixotropic agent.
Simultaneous test 1: the THIXCIN intercalation polynite thixotropic agent for preparing in the present embodiment is joined in the polyurethane sealant; Obtain the sealer product A, and the The performance test results such as the following table 1 of the sealer product B that does not add the THIXCIN intercalation polynite thixotropic agent for preparing in the present embodiment in the prior art:
The The performance test results table of table 1 simultaneous test 1
Project |
The sealer product A |
The sealer product B |
100% modulus/Mpa |
0.28 |
0.26 |
Sag (60 ℃)/mm |
2mm |
All flow out |
Sag (23 ℃)/mm |
0 |
All flow out |
This shows: use the sealer product A of the prepared THIXCIN intercalation polynite thixotropic agent of present embodiment to have good thixotropic property.
Embodiment 5
A kind of preparation method of THIXCIN intercalation polynite thixotropic agent may further comprise the steps:
Step 1, the weight part of pressing among the embodiment 2 is formed the preparation raw material;
Step 2 with 20 parts of 1 part of raw material ammonium polynite, 5 parts of THIXCINs and dry toluenes, is added in the duplicate rows star reaction kettle that the high speed dispersion dish is housed, and is warming up to 80 ℃, refluxing and stirring 3h;
Step 3, decompression vacuum pumping is removed toluene;
Step 4, temperature remain on 110 ℃, and high temperature vacuumizes 3h and removes steam;
Step 5 is cooled to 40 ℃, and 3 parts of the compsns of adding Tetra hydro Phthalic anhydride and quicklime continue to stir 0.5h, go out the still sealing, promptly get THIXCIN intercalation polynite thixotropic agent.
Simultaneous test 2: the THIXCIN intercalation polynite thixotropic agent for preparing in the present embodiment is joined in the polyurethane sealant; Obtain the sealer products C, and The performance test results such as the following table 2 of the sealer product D that does not add the THIXCIN intercalation polynite thixotropic agent for preparing in the present embodiment in the prior art:
The The performance test results table of table 2 simultaneous test 2
Project |
The sealer products C |
Sealer product D |
100% modulus/Mpa |
0.48 |
0.45 |
Sag (60 ℃)/mm |
0mm |
All flow out |
Sag (23 ℃)/mm |
0 |
10 |
This shows: use the sealer products C of the prepared THIXCIN intercalation polynite thixotropic agent of present embodiment to have good thixotropic property.
Embodiment 6
A kind of preparation method of THIXCIN intercalation polynite thixotropic agent may further comprise the steps:
Step 1, the weight part of pressing among the embodiment 3 is formed the preparation raw material;
Step 2 with 200 parts of 10 parts of raw material ammonium polynites, 18 parts of THIXCINs and dry toluenes, is added in the duplicate rows star reaction kettle that the high speed dispersion dish is housed, and is warming up to 110 ℃, refluxing and stirring 2h;
Step 3, decompression vacuum pumping is removed toluene;
Step 4, temperature remain on 115 ℃, and high temperature vacuumizes 3h and removes steam;
Step 5 is cooled to 40 ℃, adds 3 parts of Methyl benzenesulfonyl isocyanates, continues to stir 0.5h, goes out the still sealing, promptly gets THIXCIN intercalation polynite thixotropic agent.
Simultaneous test 3: the THIXCIN intercalation polynite thixotropic agent for preparing in the present embodiment is joined in the polyurethane sealant; Obtain the sealer product E, and the The performance test results such as the following table 3 of the sealer product F that does not add the THIXCIN intercalation polynite thixotropic agent for preparing in the present embodiment in the prior art:
The The performance test results table of table 3 simultaneous test 3
Project |
The sealer product E |
The sealer product F |
100% modulus/Mpa |
0.34 |
0.33 |
Sag (60 ℃)/mm |
0mm |
All flow out |
Sag (23 ℃)/mm |
0 |
17 |
This shows: use the sealer product E of the prepared THIXCIN intercalation polynite thixotropic agent of present embodiment to have good thixotropic property.
Should be noted that at last; Above embodiment is only in order to explain technical scheme of the present invention; But not to the restriction of protection domain of the present invention, although with reference to preferred embodiment the present invention has been done explanation at length, those of ordinary skill in the art is to be understood that; Can make amendment or be equal to replacement technical scheme of the present invention, and not break away from the essence and the scope of technical scheme of the present invention.