Modified molecular sieve activation powder as well as preparation method and application thereof

Abstract

The invention provides modified molecular sieve activation powder as well as a preparation method and application thereof, and belongs to the field of molecular sieve activation powder. The modified molecular sieve activation powder provided by the invention is prepared from the following raw materials in parts by mass: 40-60 parts of molecular sieve raw powder, 4-8 parts of a coupling agent, 1-10 parts of polyvinylpyrrolidone and 5-15 parts of a dispersing agent. The surface of the molecular sieve activated powder is modified by using the coupling agent in cooperation with polyvinylpyrrolidone, so that the compatibility of the molecular sieve activated powder with other components is improved, layering is avoided, the stability and storage resistance are improved, the modified molecular sieve activated powder with high compatibility with the coating is finally prepared, and the modified molecular sieve activated powder has flowability and can be used for preparing the coating. And the activated powder is uniformly dispersed in the coating, is simple to use and operate, and is prevented from drifting in the air to influence the environment.

Description

Technical Field

[0001] The invention relates to the field of molecular sieve activation powder, and in particular to a modified molecular sieve activation powder and a preparation method and application thereof. Background Art

[0002] Molecular sieve is a kind of aluminosilicate, which is mainly composed of silicon and aluminum connected by oxygen bridges to form an open skeleton structure. There are many channels with uniform pore size and neatly arranged holes with large internal surface area in the structure. There are many cavities of the same size inside, and the cavities are connected by many micropores of the same diameter. The molecules of substances smaller than the diameter of the channels are adsorbed inside the cavities, while the molecules larger than the channels are excluded, so that molecules of different sizes and shapes are separated, which plays the role of screening molecules, so it is called molecular sieve.

[0003] Molecular sieve activation powder is a molecular sieve obtained by dehydrating the original molecular sieve synthesis powder. It has good dispersibility and fast adsorption speed and is used in some special adsorption occasions in industry, such as mixed dispersion adsorption with materials as amorphous desiccant, etc. It is specifically used as an additive or material for coatings, paints, resins and certain adhesives, and has the effects of reducing moisture, eliminating bubbles, and improving the uniformity and strength of materials. The traditional method is to add powdered molecular sieve activation powder directly to the coating, which is prone to uneven dispersion, complicated operation, and part of the activated powder powder will float in the air, resulting in a waste of raw materials and high dust pollution, and the working environment is relatively poor. In order to solve this problem, the prior art prepares a paste-like molecular sieve activation powder, but the paste-like molecular sieve activation powder has poor compatibility with the coating, and the paste-like molecular sieve activation powder is easy to stratify and has poor storage resistance. Summary of the invention

[0004] The object of the present invention is to provide a modified molecular sieve activation powder and a preparation method thereof. The modified molecular sieve activation powder prepared by the method provided by the present invention has good compatibility with coatings, is not easy to delaminate, and has excellent stability and storage resistance.

[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0006] The invention provides a modified molecular sieve activation powder, which is prepared by comprising the following raw materials, by weight: 40 to 60 parts of molecular sieve original powder, 4 to 8 parts of coupling agent, 1 to 10 parts of polyvinyl pyrrolidone, and 5 to 15 parts of dispersant.

[0007] Preferably, the following raw materials are included in the preparation, calculated by weight: 45 to 58 parts of molecular sieve powder, 5 to 8 parts of coupling agent, 2 to 8 parts of polyvinyl pyrrolidone, and 7 to 13 parts of dispersant.

[0008] Preferably, the molecular sieve raw powder is 3A or 4A molecular sieve raw powder.

[0009] Preferably, the coupling agent is at least one of KH-540, KH-550, and KH-560.

[0010] Preferably, the dispersant is at least one of propylene glycol, butylene glycol, diethylene glycol and triethylene glycol.

[0011] The present invention also provides a method for preparing the modified molecular sieve activation powder described in the above technical solution, comprising the following steps:

[0012] (1) mixing molecular sieve raw powder and alcohol solvent, adding coupling agent, and sequentially performing first stirring treatment and post-treatment to obtain modified molecular sieve raw powder;

[0013] The modified molecular sieve raw powder is subjected to vacuum heat treatment and cooling to obtain pretreated molecular sieve activated powder;

[0014] (2) In an inert atmosphere, the pretreated molecular sieve activation powder obtained in step (1) is mixed with polyvinyl pyrrolidone and a dispersant, and subjected to a second stirring treatment to obtain a modified molecular sieve activation powder.

[0015] Preferably, the temperature of the first stirring treatment in step (1) is 40 to 60° C., and the time of the first stirring treatment is 1 to 5 hours.

[0016] Preferably, the temperature of the vacuum heat treatment in step (1) is 380-500° C., and the time of the vacuum heat treatment is 20-60 min.

[0017] Preferably, the temperature of the second stirring treatment in step (2) is 30 to 50° C., and the time of the second stirring treatment is 1 to 3 hours.

[0018] The present invention also provides the use of the modified molecular sieve activation powder described in the above technical solution or the modified molecular sieve activation powder prepared by the preparation method in coatings.

[0019] The present invention provides a modified molecular sieve activation powder, which is prepared by including the following raw materials by weight: 40 to 60 parts of molecular sieve original powder, 4 to 8 parts of coupling agent, 1 to 10 parts of polyvinyl pyrrolidone, and 5 to 15 parts of dispersant. The present invention uses coupling agent and polyvinyl pyrrolidone to modify the surface of molecular sieve activation powder to improve its compatibility with other components, avoid stratification, improve stability and storage resistance, and finally prepare modified molecular sieve activation powder with high compatibility with coatings, and the modified molecular sieve activation powder has fluidity, is evenly dispersed in the coating, is simple to use and operate, and avoids the activation powder powder floating in the air and affecting the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1It is a statistical graph of the static water adsorption rate of the modified molecular sieve activation powder prepared in Examples 1 to 6 of the present invention and the molecular sieve activation powder prepared in Comparative Examples 1 to 4. DETAILED DESCRIPTION

[0021] The invention provides a modified molecular sieve activation powder, which is prepared by comprising the following raw materials, by weight: 40 to 60 parts of molecular sieve original powder, 4 to 8 parts of coupling agent, 1 to 10 parts of polyvinyl pyrrolidone, and 5 to 15 parts of dispersant.

[0022] In the present invention, the modified molecular sieve activation powder is preferably prepared by the following raw materials, calculated by weight: 45-58 parts of molecular sieve original powder, 5-8 parts of coupling agent, 2-8 parts of polyvinyl pyrrolidone, and 7-13 parts of dispersant. The present invention controls the amount of each component within the above range to achieve a better surface modification effect on the molecular sieve activation powder, and obtains a modified molecular sieve activation powder with high compatibility with the coating, high stability, and not easy to delaminate.

[0023] In the present invention, the molecular sieve raw powder is preferably 3A molecular sieve raw powder or 4A molecular sieve raw powder.

[0024] In the present invention, the coupling agent is preferably at least one of KH-540, KH-550 and KH-560.

[0025] In the present invention, the dispersant is preferably at least one of propylene glycol, butylene glycol, diethylene glycol and triethylene glycol. The present invention utilizes the dispersant to improve the storage stability of the prepared modified molecular sieve activation powder and its dispersion stability in the coating.

[0026] The present invention also provides a method for preparing the modified molecular sieve activation powder described in the above technical solution, comprising the following steps:

[0027] (1) mixing molecular sieve raw powder and alcohol solvent, adding coupling agent, and sequentially performing first stirring treatment and post-treatment to obtain modified molecular sieve raw powder;

[0028] The modified molecular sieve raw powder is subjected to vacuum heat treatment and cooling to obtain pretreated molecular sieve activated powder;

[0029] (2) In an inert atmosphere, the pretreated molecular sieve activation powder obtained in step (1) is mixed with polyvinyl pyrrolidone and a dispersant, and subjected to a second stirring treatment to obtain a modified molecular sieve activation powder.

[0030] The invention mixes molecular sieve raw powder and alcohol solvent, then adds coupling agent, and sequentially performs first stirring treatment and post-treatment to obtain modified molecular sieve raw powder.

[0031] In the present invention, the alcohol solvent is preferably ethanol; the mass ratio of the molecular sieve raw powder to the alcohol solvent is preferably (1-3):10.

[0032] In the present invention, the temperature of the first stirring treatment is preferably 40-60°C, and the time of the first stirring treatment is preferably 1-5 hours. The present invention controls the temperature and time of the first stirring treatment within the above range to fully achieve the surface modification of the molecular sieve raw powder by the coupling agent.

[0033] In the present invention, the post-treatment preferably includes: centrifuging, washing and drying the product of the first stirring treatment in sequence to obtain modified molecular sieve raw powder.

[0034] The present invention realizes solid-liquid separation by centrifugation. The present invention has no special restrictions on the washing and drying methods, and only needs to remove the residual solvent.

[0035] After obtaining the modified molecular sieve raw powder, the present invention performs vacuum heat treatment and cooling on the modified molecular sieve raw powder to obtain pretreated molecular sieve activated powder.

[0036] In the present invention, the temperature of the vacuum heat treatment is preferably 380-500°C, and the time of the vacuum heat treatment is preferably 20-60 minutes. The present invention controls the temperature and time of the vacuum heat treatment within the above range to promote the full activation of the modified molecular sieve raw powder and remove moisture. In the present invention, the water content of the pretreated molecular sieve activated powder is preferably ≤0.5%. In the present invention, the cooling is preferably carried out in an inert atmosphere or vacuum.

[0037] After obtaining the pretreated molecular sieve activation powder, the present invention mixes the pretreated molecular sieve activation powder with polyvinyl pyrrolidone and a dispersant in an inert atmosphere, and performs a second stirring treatment to obtain a modified molecular sieve activation powder.

[0038] In the present invention, the temperature of the second stirring treatment is preferably 30-50°C, and the time of the second stirring treatment is preferably 1-3 hours. The present invention promotes uniform mixing of the components through the second stirring treatment, achieves a better modification effect, and obtains a modified molecular sieve activation powder with good comprehensive performance.

[0039] The present invention also provides the application of the modified molecular sieve activation powder described in the above technical solution or the modified molecular sieve activation powder prepared by the preparation method in coatings.

[0040] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0041] Example 1

[0042] A modified molecular sieve activation powder is prepared from the following raw materials, calculated by weight: 48 parts of 3A molecular sieve original powder, 6 parts of coupling agent (KH-560), 2 parts of polyvinyl pyrrolidone, and 13 parts of dispersant butanediol.

[0043] The preparation method of the modified molecular sieve activated powder comprises the following steps:

[0044] (1) Mixing 3A molecular sieve raw powder and ethanol at a mass ratio of 1:10, adding coupling agent KH-560, stirring for the first time at 55° C. for 1.5 h, and then centrifuging, washing and drying in sequence to obtain modified molecular sieve raw powder;

[0045] The modified molecular sieve raw powder is subjected to vacuum heat treatment at 400° C. for 40 minz, and cooled in a nitrogen atmosphere to obtain a pretreated molecular sieve activated powder;

[0046] (2) In a nitrogen atmosphere, the pretreated molecular sieve activation powder obtained in step (1) is mixed with polyvinyl pyrrolidone and a dispersant, and a second stirring treatment is performed at 40° C. for 2 h to obtain a modified molecular sieve activation powder.

[0047] Example 2

[0048] A modified molecular sieve activation powder is prepared from the following raw materials, calculated by weight: 48 parts of 3A molecular sieve original powder, 7 parts of coupling agent KH-560, 4 parts of polyvinyl pyrrolidone, and 13 parts of dispersant butanediol.

[0049] The modified molecular sieve activation powder was prepared according to the method of Example 1.

[0050] Example 3

[0051] A modified molecular sieve activation powder is prepared from the following raw materials, calculated by weight: 48 parts of 3A molecular sieve original powder, 7 parts of coupling agent KH-560, 6 parts of polyvinyl pyrrolidone, and 13 parts of dispersant diethylene glycol.

[0052] The modified molecular sieve activation powder was prepared according to the method of Example 1.

[0053] Example 4

[0054] A modified molecular sieve activation powder is prepared from the following raw materials, calculated by weight: 48 parts of 3A molecular sieve original powder, 7 parts of coupling agent KH-560, 8 parts of polyvinyl pyrrolidone, and 13 parts of dispersant diethylene glycol.

[0055] The modified molecular sieve activation powder was prepared according to the method of Example 1.

[0056] Example 5

[0057] A modified molecular sieve activation powder is prepared from the following raw materials, calculated by weight: 48 parts of 4A molecular sieve original powder, 7 parts of coupling agent KH-560, 6 parts of polyvinyl pyrrolidone, and 13 parts of dispersant triethylene glycol.

[0058] The modified molecular sieve activation powder was prepared according to the method of Example 1.

[0059] Example 6

[0060] A modified molecular sieve activation powder is prepared from the following raw materials, calculated by weight: 48 parts of 4A molecular sieve original powder, 7 parts of coupling agent KH-560, 8 parts of polyvinyl pyrrolidone, and 13 parts of dispersant triethylene glycol.

[0061] The modified molecular sieve activation powder was prepared according to the method of Example 1.

[0062] Comparative Example 1

[0063] The 3A molecular sieve raw powder was subjected to vacuum heat treatment at 400° C. for 40 minz, and cooled in a nitrogen atmosphere to obtain a molecular sieve activated powder.

[0064] Comparative Example 2

[0065] Molecular sieve activation powder was prepared according to the method of Example 1, except that no coupling agent was added.

[0066] Comparative Example 3

[0067] Molecular sieve activation powder was prepared according to the method of Example 1, except that polyvinyl pyrrolidone was not added.

[0068] Comparative Example 4

[0069] Molecular sieve activation powder was prepared according to the method of Example 1, except that polyvinyl pyrrolidone was not added.

[0070] According to the GB6287-86 molecular sieve static water adsorption determination method, at 10% humidity and 25°C, the 72h static water adsorption rates of the modified molecular sieve activation powders prepared in Examples 1 to 6 and the molecular sieve activation powders prepared in Comparative Examples 1 to 4 were respectively measured. The results are shown in Tables 1 and Figure 1 shown.

[0071] Dispersibility test: castor oil was used as a medium, and samples prepared in the embodiment and the comparative example were added at room temperature of 25-30°C, with a mass ratio of castor oil: sample = 3:1. The mixture was stirred at 1000rpm for 15min until uniform and then allowed to stand for observation. The stirring step was repeated every other week. The temperature was kept at 25-30°C and the relative humidity was 50-60%. After 8 weeks, it was observed whether there was obvious particle sedimentation, scattered particles, or whether the stirring rod was stuck with sample molecular sieve particles. If any of these items appeared, it was recorded as unqualified. On the contrary, if none of these items appeared, it was qualified. 50 samples were tested in each group to obtain the sample qualified rate, and the results were recorded in Table 1.

[0072] Table 1 Statistics of static water adsorption rate and dispersion qualification rate of the modified molecular sieve activation powder prepared in Examples 1 to 6 and the molecular sieve activation powder prepared in Comparative Examples 1 to 4

[0073]

[0074]

[0075] Example 7

[0076] The modified molecular sieve activation powder was prepared according to the method of Example 1, except that the temperature of the vacuum heat treatment in step (1) was 420°C.

[0077] Example 8

[0078] The modified molecular sieve activation powder was prepared according to the method of Example 1, except that the temperature of the vacuum heat treatment in step (1) was 450°C.

[0079] Example 9

[0080] The modified molecular sieve activation powder was prepared according to the method of Example 1, except that the temperature of the second stirring treatment in step (2) was 30°C.

[0081] Example 10

[0082] The modified molecular sieve activation powder was prepared according to the method of Example 1, except that the temperature of the second stirring treatment in step (2) was 30° C. and the time of the second stirring treatment was 1 h.

[0083] Embodiment 11

[0084] The modified molecular sieve activation powder was prepared according to the method of Example 1, except that the temperature of the second stirring treatment in step (2) was 50°C.

[0085] In summary, compared with the comparative example, the static water adsorption rate of the modified molecular sieve activation powder prepared by the method provided by the present invention in Examples 1 to 6 is equivalent, and the dispersibility is excellent, indicating that the adsorption capacity of the modified molecular sieve activation powder prepared in Examples 1 to 6 is not affected, and is slightly increased, with good stability and storage resistance. At the same time, the present invention also measured the static water adsorption rate of the modified molecular sieve activation powder prepared in Examples 7 to 11, and the test results were all greater than 20%, and the dispersibility qualified rate was 100%.

[0086] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A modified molecular sieve activation powder, characterized in that: The preparation method comprises the following raw materials, calculated by weight: 40 to 60 parts of molecular sieve powder, 4 to 8 parts of coupling agent, 1 to 10 parts of polyvinyl pyrrolidone and 5 to 15 parts of dispersant.

2. The modified molecular sieve activation powder according to claim 1, characterized in that: The preparation method comprises the following raw materials, calculated by weight: 45 to 58 parts of molecular sieve powder, 5 to 8 parts of coupling agent, 2 to 8 parts of polyvinyl pyrrolidone and 7 to 13 parts of dispersant.

3. The modified molecular sieve activation powder according to claim 1 or 2, characterized in that: The molecular sieve raw powder is 3A molecular sieve raw powder or 4A molecular sieve raw powder.

4. The modified molecular sieve activation powder according to claim 1 or 2, characterized in that: The coupling agent is at least one of KH-540, KH-550 and KH-560.

5. The modified molecular sieve activation powder according to claim 1 or 2, characterized in that: The dispersant is at least one of propylene glycol, butylene glycol, diethylene glycol and triethylene glycol.

6. The method for preparing the modified molecular sieve activation powder according to any one of claims 1 to 5, characterized in that: The following steps are involved: (1) mixing molecular sieve raw powder and alcohol solvent, adding coupling agent, and sequentially performing first stirring treatment and post-treatment to obtain modified molecular sieve raw powder; The modified molecular sieve raw powder is subjected to vacuum heat treatment and cooling to obtain pretreated molecular sieve activated powder; (2) In an inert atmosphere, the pretreated molecular sieve activation powder obtained in step (1) is mixed with polyvinyl pyrrolidone and a dispersant, and subjected to a second stirring treatment to obtain a modified molecular sieve activation powder.

7. The method for preparing the modified molecular sieve activation powder according to claim 6, characterized in that: The temperature of the first stirring treatment in step (1) is 40 to 60° C., and the time of the first stirring treatment is 1 to 5 hours.

8. The method for preparing the modified molecular sieve activation powder according to claim 6, characterized in that: The temperature of the vacuum heat treatment in step (1) is 380-500° C., and the time of the vacuum heat treatment is 20-60 minutes.

9. The method for preparing the modified molecular sieve activation powder according to claim 6, characterized in that: The temperature of the second stirring treatment in step (2) is 30 to 50° C., and the time of the second stirring treatment is 1 to 3 hours.

10. The modified molecular sieve activation powder according to any one of claims 1 to 5 Or use of the modified molecular sieve activated powder prepared by the preparation method according to any one of claims 6 to 9 in coatings.

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