A kind of synthetic method of hydrophobic calcium sulfate hemihydrate of water resistance

A technology of calcium sulfate hemihydrate and a synthesis method, which is applied in the field of synthesis of hydrophobic calcium sulfate hemihydrate whiskers, can solve problems such as unsuitable dispersion, and achieve the effects of easy popularization, easy availability and wide application range.

Active Publication Date: 2019-04-05
QINGDAO UNIV OF SCI & TECH
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Problems solved by technology

Based on the silane coupling agent KH570, one end is a silicon hydroxyl group, which can be grafted with the hydroxyl group on the surface of the whisker due to hydrogen bonding, and one end has a double bond. The introduction of a mercapto compound through a mercapto-ene reaction can not only prepare a water-resistant hydrophobic Calcium sulfate hemihydrate whiskers can introduce mercapto compounds at the same time, improving the disadvantages of inorganic whisker materials that are not suitable for dispersion when used as fillers

Method used

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  • A kind of synthetic method of hydrophobic calcium sulfate hemihydrate of water resistance
  • A kind of synthetic method of hydrophobic calcium sulfate hemihydrate of water resistance
  • A kind of synthetic method of hydrophobic calcium sulfate hemihydrate of water resistance

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[0033] The invention provides a kind of synthetic method of the hydrophobic calcium sulfate hemihydrate of preparation water resistance, comprising:

[0034] Silane coupling agent KH570 modified calcium sulfate hemihydrate whisker, the reaction mechanism is as follows:

[0035]

[0036] Because the grafting reaction of the silane coupling agent KH570 relies on the hydrogen bond between the silicon hydroxyl group and the whisker surface hydroxyl group, the grafting rate is low. Therefore, the present invention has carried out systematic research and experimental exploration on the reaction temperature of the grafting reaction, the reaction time and the proportion of reactants, and proposes to graft and introduce the silane coupling agent KH570 on the terminal hydroxyl groups on the surface of the whiskers to utilize the hydroxyl and silicon Hydrogen bonding takes place in the hydroxyl group to block the end group, which effectively prevents the hydroxyl group on the whisker ...

Embodiment 1

[0054] Weigh 5g of calcium sulfate hemihydrate whiskers and disperse in 100mL of absolute ethanol for 1h, adjust pH=3.5, and record it as solution A; weigh an equivalent amount of KH570 and dissolve in 30mL of ethanol solution (alcohol-water ratio is 3:1), Adjust the pH to 3.5, hydrolyze for 20 minutes, and record it as solution B; then slowly add solution B dropwise to solution A, react at 50°C for 1-5 hours, filter with suction, dry, and measure the contact angle of whiskers after the reaction. The measured contact angle angles are shown in Table 1, the best reaction time is 4h, and the contact angle at this time is 18.83°

Embodiment 2

[0056] Weigh 5g of calcium sulfate hemihydrate whiskers and disperse in 100mL of absolute ethanol for 1h, adjust pH=3.5, and record it as solution A; weigh an equivalent amount of KH570 and dissolve in 30mL of ethanol solution (alcohol-water ratio is 3:1), Adjust the pH to 3.5, hydrolyze for 20 minutes, and record it as solution B; then slowly add solution B dropwise to solution A, react at 40-80°C for 4 hours, filter with suction, dry, and measure the contact angle of whiskers after the reaction. The measured contact angle angles are shown in Table 2. The optimum reaction temperature is 70°C, and the contact angle at this time is 36.61°

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Abstract

The invention provides a synthesis method of hydration-resistant hydrophobic calcium sulfate hemihydrate. The synthesis method comprises the following steps: leading calcium sulfate hemihydrate whisker, prepared by using the traditional hydrothermal method, and a silane coupling agent KH570 to be subjected to hydrogen-bond interaction to obtain calcium sulfate hemihydrate whisker with KH570-grafted surfaces, then leading the whisker and trimethylolpropanetri(3-thiohydracrylic acid)ester (TTMP) to generate thiol-ene photo-curing reaction to obtain secondarily modified calcium sulfate hemihydrate whisker which is hydration-resistant hydrophobic calcium sulfate hemihydrate whisker. The synthesis method of the hydration-resistant hydrophobic calcium sulfate hemihydrate whisker is novel, simplein steps, fast to react and beneficial to environment protection, has wide market prospects. The synthesis method has simple steps, and is simple to operate and strong in practicability.

Description

technical field [0001] The invention belongs to the field of preparation of calcium sulfate hemihydrate whiskers, in particular to a method for synthesizing water-resistant hydrophobic calcium sulfate hemihydrate whiskers. Background technique [0002] Calcium sulfate is a naturally occurring common inorganic compound that plays a very important role in industrial production. At present, its main form in nature is large mineral gypsum (calcium sulfate dihydrate, CaSO 4 2H 2 O) and anhydrite (anhydrous calcium sulfate) in two forms. In addition, calcium sulfate also exists in other forms. Calcium sulfate hemihydrate whiskers have many advantages such as high strength, low cost, non-toxicity, and environmental protection because of their special physical and chemical properties, and are widely used in plastics. , rubber and other fields. However, calcium sulfate hemihydrate whiskers are very sensitive to air and water, and are easily hydrated at room temperature. After hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/06C08K9/04C08K7/08C08L83/04
Inventor 高传慧王博任秀王汇淄刘月涛王静武玉民
Owner QINGDAO UNIV OF SCI & TECH
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