TEMPORARY HIGH-TEMPERATURE-RESISTANT DISPERSING AGENT AND PREPARATION AND USE METHOD THEREOF

Abstract

A temporary high-temperature-resistant dispersing agent, and a preparation and a use method thereof. The temporary high-temperature-resistant dispersing agent is a block high-molecular polymer prepared by a one-step reaction from polysiloxane containing an amino group. The prepared block high-molecular polymer may be directly used as a dispersant; the block high-molecular polymer may also be used as a basic formula and used as the dispersant after other auxiliary compositions are added; and the block high-molecular polymer may also be used in combination with one or more other dispersion auxiliaries and/or surfactants to meet dispersion requirements in various special occasions.

Claims

1. A preparation of a temporary high-temperature-resistant dispersing agent, comprising the following steps: under the condition of using a solvent or not using the solvent, obtaining the temporary high-temperature-resistant dispersing agent through a Mannich reaction by mixing an organosilicon compound containing two amino groups, an aldehyde (ketone) compound and an organic compound containing two phenolic hydroxyl groups.

2. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein the organosilicon compound containing two amino groups is a compound containing two or more amino groups and one or more siloxy groups in a molecular structure.

3. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 2, wherein the organosilicon compound containing two amino groups is small molecule siloxane containing two or more amino groups in the molecular structure, oligosiloxane containing two or more amino groups in the molecular structure, polysiloxane containing two or more amino groups in the molecular structure, silicone resin containing two or more amino groups in the molecular structure, silicone rubber containing two or more amino groups in the molecular structure, a block copolymer of siloxane and other polymers containing two or more amino groups in the molecular structure or a graft copolymer of siloxane and other polymers containing two or more amino groups in the molecular structure.

4. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein the aldehyde (ketone) compound is a small molecule aldehyde (ketone) compound able to be dissolved in a reaction system.

5. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 4, wherein the aldehyde (ketone) compound is formaldehyde, acetone, benzaldehyde, trioxymethylene, paraformaldehyde or cyclohexanone.

6. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein the organic compound containing two phenolic hydroxyl groups is an organic compound whose molecular structure at least contains two phenolic hydroxyl groups that are not on the same benzene ring.

7. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 6, wherein the organic compound containing two phenolic hydroxyl groups is bisphenol A, dihydroxy diphenyl ether, dihydroxy benzophenone, bisphenol F, bisphenol S, 2,2-diallyl bisphenol A, dihydroxybiphenyl or bisphenol fluorene.

8. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein the solvent is various polar or nonpolar solvents that are able to dissolve a reactant without having a chemical reaction with the reactant.

9. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 8, wherein the solvent is dioxane, toluene, tetrahydrofuran, chloroform, methanol, ethanol, diphenyl ether, dimethyl sulfoxide or N,N-dimethylformamide.

10. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein a material molar ratio of the organosilicon compound containing two amino groups to the aldehyde (ketone) compound to the organic compound containing two phenolic hydroxyl groups is 1: (1-20):(1-20).

11. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 10, wherein a material molar ratio of the organosilicon compound containing two amino groups to the aldehyde (ketone) compound to the organic compound containing two phenolic hydroxyl groups is 1: (4-15):(1-10).

12. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein a reaction temperature of the organosilicon compound containing two amino groups, the aldehyde (ketone) compound and the organic compound containing two phenolic hydroxyl groups is 30-180 C.

13. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 12, wherein a reaction temperature of the organosilicon compound containing two amino groups, the aldehyde (ketone) compound and the organic compound containing two phenolic hydroxyl groups is 40-80 C.

14. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 1, wherein reaction time of the organosilicon compound containing two amino groups, the aldehyde (ketone) compound and the organic compound containing two phenolic hydroxyl groups is 1-60 h.

15. The preparation of the temporary high-temperature-resistant dispersing agent according to claim 14, wherein reaction time of the organosilicon compound containing two amino groups, the aldehyde (ketone) compound and the organic compound containing two phenolic hydroxyl groups is 12-24 h.

16. A temporary high-temperature-resistant dispersing agent prepared by the method according to claim 1.

17. A use method of the temporary high-temperature-resistant dispersing agent according to claim 16, comprising the following steps: directly serving as a dispersant to be used; or adding a catalyst, a filler and an auxiliary to be used cooperatively; or using in combination with one or more other dispersion auxiliaries and/or surfactants.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0028] FIG. 1 is a nuclear magnetic spectrogram of a block polymer dispersant containing fluorenyl obtained by Embodiment 2.

[0029] FIG. 2 is an infrared spectrogram of a block polymer dispersant containing fluorenyl obtained by Embodiment 2.

[0030] FIG. 3 is a TGA diagram of a block polymer dispersant containing fluorenyl obtained by Embodiment 2.

DETAILED DESCRIPTION OF THE EMBODIMENTS

[0031] The present disclosure is further explained by specific embodiments below, but is not limited to this.

[0032] Raw materials used in the embodiments are all conventional commercially purchased raw materials or obtained through synthesis according to methods in references.

[0033] A molar ratio in the embodiments is a proportion of the amount of substances and a proportion of parts is a mass proportion.

Embodiment 1

[0034] Aminopropyl-terminated disiloxane, bisphenol fluorene and trioxymethylene are evenly mixed in toluene according to a molar ratio of 1:1.5:4, kept at 80 C., and mechanically stirred for 6 hours to obtain a block polymer dispersant containing fluorenyl. The yield of the block polymer dispersant containing fluorenyl is 85%.

Embodiment 2

[0035] As described in Embodiment 1, the differences are that the aminopropyl-terminated disiloxane is changed to aminopropyl-terminated polysiloxane (number-average molecular weight is 5000), the trioxymethylene is changed to a formaldehyde aqueous solution (the concentration of formaldehyde aqueous solution is 37 wt %), and the molar ratio is changed to 1:1:6. The reaction temperature is changed to 70 C., mechanical stirring is performed for 12 hours, and a block polymer dispersant containing fluorenyl is obtained, the reaction yield of the block polymer dispersant containing fluorenyl is 97%.

[0036] Hydrogen nuclear magnetic resonance of the block polymer dispersant synthesized in the embodiment is as shown in FIG. 1, .sup.1H NMR (CDCl.sub.3):=0.05 ppm is the peak location of hydrogen in silylmethyl (SiCH.sub.3) in siloxane, =0.51 ppm is the peak location of the first methylene (SiCH.sub.2CH.sub.2CH.sub.2N) connected to silicon, =1.53 ppm is the peak location of the second methylene (SiCH.sub.2CH.sub.2CH.sub.2N) connected to silicon, =2.66 ppm is the peak location of the third methylene (SiCH.sub.2CH.sub.2CH.sub.2N) connected to silicon, =3.74 ppm is the peak location of ArCH.sub.2N, =4.74 ppm is the peak position of OCH.sub.2N, and between 6.65-7.76 ppm is the peak position of hydrogen on a benzene ring (ArH).

[0037] An infrared representation of the block polymer dispersant synthesized in the embodiment is as shown in FIG. 2. It can be seen from FIG. 2 that peaks of 1055 cm.sup.1 and 1022 cm.sup.1 are generated by asymmetric bending vibration of SiOSi in polysiloxane. 1261 cm.sup.1 and 1183 cm.sup.1 are asymmetric stretching vibration peaks of COC and CNC on an oxazine ring respectively. 935 cm.sup.1 is a characteristic absorption peak of a benzene ring connected with the oxazine ring, that is, the characteristic absorption peak of the oxazine ring, indicating that benzoxazine has been generated; and similarly, there are also peaks at 1495 cm.sup.1 and 719 cm.sup.1, indicating that the 1,2,4 triple substituted peaks of the benzene ring has been generated, which further explains the generation of the oxazine ring.

[0038] TGA test results of the block polymer dispersant synthesized in the embodiment are as shown in FIG. 3: it can be seen from FIG. 3 that the temperature of a 5% thermal weight loss is 325 C., and the char yield at 600 C. is only 7%. It indicates that the substance is still stable when heated to 300 C., but almost no longer exists when heated to 600 C., that is, the substance may be removed by heating.

[0039] A reaction process of the block polymer dispersant obtained in the embodiment is as follows:

##STR00002##

Embodiment 3

[0040] As described in Embodiment 2, the difference is that the bisphenol fluorene is changed to bisphenol A, other parameters are the same, and a block polymer dispersant containing a bisphenol A structure is obtained, the reaction yield of the block polymer dispersant containing a bisphenol A structure is 100%.

Embodiment 4

[0041] As described in Embodiment 2, the difference is that the bisphenol fluorene is changed to bisphenol S, and a block polymer dispersant containing bisphenol S is finally obtained, the reaction yield of the block polymer dispersant containing bisphenol S reaching 100%.

Embodiment 5

[0042] As described in Embodiment 2, the difference is that the bisphenol fluorene is changed to 2,2-diallyl bisphenol A. A block polymer dispersant containing bisphenol A is finally obtained, and the reaction yield of the block polymer dispersant containing bisphenol A reaches 90%.

Embodiment 6

[0043] As described in Embodiment 2, the difference is that the aminopropyl-terminated polysiloxane (number-average molecular weight is 5000) is changed to aminopropyl-terminated polysiloxane (number-average molecular weight is 10000), a product is a block polymer dispersant containing fluorenyl benzoxazine, and the reaction yield of the block polymer dispersant containing fluorenyl benzoxazine reaches 96%.

Embodiment 7

[0044] As described in Embodiment 6, the difference is that the bisphenol fluorene is changed to bisphenol S, a product is a block polymer dispersant containing bisphenol S, and the reaction yield of the block polymer dispersant containing bisphenol S is 96%.

Embodiment 8

[0045] As described in Embodiment 6, the difference is that the bisphenol fluorene is changed to 2,2-diallyl bisphenol A, and a solvent is changed to chloroform. A product is a block polymer dispersant containing fluorenyl, and the reaction yield of the block polymer dispersant containing fluorenyl is 93%.

Embodiment 9

[0046] As described in Embodiment 8, the difference is that a formaldehyde aqueous solution is changed to paraformaldehyde, and a solvent is changed to tetrahydrofuran. A product is a block polymer dispersant containing fluorenyl, and the reaction yield of the block polymer dispersant containing fluorenyl is 96%.

Embodiment 10

[0047] As described in Embodiment 2, the difference is that acetic acid is added to serve as a catalyst of a reaction, the adding amount is 5% of the amount of substance of the aminopropyl-terminated polysiloxane, and reaction time is 3 hours. A product is a block polymer dispersant containing fluorenyl, and the reaction yield of the block polymer dispersant containing fluorenyl is 94%.

Embodiment 11

[0048] The block polymer dispersant containing fluorenyl obtained in Embodiment 2 is used as a basic formula (100 parts), methylsilicone oil (10 parts) with the type of 201 is added for compounding, and uniform mixing is performed. Then, temperature resistance performance of the dispersant is determined.

Embodiment 12

[0049] The block polymer dispersant obtained in Embodiment 6 is used as a basic formula (100 parts), 10 parts of high temperature conduction oil are added, and uniform mixing is performed. Then, temperature resistance performance of the dispersant is determined.

Test Example 1

[0050] The heat resistance of the dispersants in Embodiments 2, 3, 11 and 12 is tested. The dispersibility is determined in accordance with the industry standard HG/T2499-2006, and results are as shown in Table 1.

TABLE-US-00001 TABLE 1 Dispersibility Embodi- Experimental Experimental Sample (of standard ments time temperature appearance substances) % Embodiment 2 h 280 C. Pale yellow 120 2 oiliness Embodiment 1.8 h 290 C. Pale yellow 118 3 oiliness Embodiment 2.5 h 300 C. Pale yellow 106 11 oiliness Embodiment 2.3 h 275 C. Pale yellow 109 12 oiliness

[0051] It can be seen from Table 1 that the block polymer dispersant prepared in the present disclosure may be used as a dispersant itself and has high-temperature resistance. When such dispersant is mixed with other auxiliaries for compounding, the performance is still very good, and the overall temperature resistance performance is even higher than temperature resistance data of a high-temperature resistant dispersant reported in the references. The data show that the dispersant of the present disclosure has obvious superiority in temperature resistance performance. In combination with the above-mentioned advantages of the present disclosure in preparation process, the creativity of the present disclosure is further demonstrated.

[0052] It can be seen from FIG. 3 that a 5% thermal weight loss of the block polymer dispersant in Embodiment 2 is at 380 C., and a 10% thermal weight loss is at 450 C. This indicates that the dispersant may be used at the temperature below 450 C. and has good temperature resistance. It can also be seen from FIG. 3 that when the temperature rises to be above 450 C., the block polymer dispersant begins to decompose rapidly. When the temperature rises to 550 C., the mass of residual char of the block polymer dispersant is about 10%, showing good temporary performance.