Polyether calcium phosphate quantum dot and preparation method thereof

文档序号:845686 发布日期:2021-03-16 浏览:5次 中文

阅读说明:本技术 聚醚磷酸钙量子点及其制备方法 (Polyether calcium phosphate quantum dot and preparation method thereof ) 是由 程亮 于 2020-12-09 设计创作,主要内容包括:本发明公开了一种聚醚磷酸钙量子点及其制备方法,所述量子点是由聚醚与磷酸钙组成,其中聚醚为壳层,磷酸钙为核心。制备方法:将氢氧化钙配成去离子水-乙醇溶液,在40℃条件下,将磷酸和聚醚同时加入到氢氧化钙溶液中,添加过程中始终控制Ca~(2+):PO_3~(3-)摩尔比保持3:2,滴加完成继续反应0.5-3小时,过滤,得到粘稠状固体;干燥1-5小时,得到目标产品。本发明是一种新型量子点,该量子点颗粒均匀、与水和油均具有良好的分散性,在油品中具有良好的抗磨性。(The invention discloses a polyether calcium phosphate quantum dot and a preparation method thereof. The preparation method comprises the following steps: preparing calcium hydroxide into deionized water-ethanol solution, and treating at 40 deg.CAdding phosphoric acid and polyether into calcium hydroxide solution at the same time, and controlling Ca all the time in the adding process 2+ :PO 3 3‑ Keeping the molar ratio at 3:2, continuously reacting for 0.5-3 hours after the dropwise adding is finished, and filtering to obtain a viscous solid; drying for 1-5 hours to obtain the target product. The invention is a novel quantum dot, the quantum dot particles are uniform, have good dispersibility with water and oil, and have good abrasion resistance in oil products.)

1. The polyether calcium phosphate quantum dot is characterized by consisting of polyether and calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

2. The polyether calcium phosphate quantum dot of claim 1, wherein the polyether is selected from a water-soluble polyether, a water-insoluble polyether, or an oil-soluble polyether.

3. The polyether calcium phosphate quantum dot of claim 2, wherein the polyether is a compound of the following formula:

wherein m is 0 to 100, n is 0 to 100, m and n are not zero at the same time, and R is1Is C1~C30Of (a) an alkane. R2Is hydrogen or methyl, R3Is C2~C30Of (a) an alkane.

4. The polyethercalcium phosphate quantum dot of claim 3, wherein R is1Is C1~C10Of (a) an alkane.

5. The polyethercalcium phosphate quantum dot of claim 3, wherein R is3Is C2~C20Of (a) an alkane.

6. The calcium phosphate polyether quantum dot of claim 1, wherein the quantum dot particle diameter is less than 10 nm.

7. The preparation method of the polyether calcium phosphate quantum dot is characterized by comprising the following steps:

A. weighing the following raw materials: 40-50 parts of polyether, 40-50 parts of calcium hydroxide, 40-50 parts of phosphoric acid, a proper amount of deionized water and a proper amount of ethanol;

B. preparing calcium hydroxide into 0.01-2.0mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at 40 deg.C at 0.1-2.0 mL/min, and controlling Ca concentration during the addition process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 0.5-3 hours after the dropwise addition is finished to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid;

D. drying the viscous solid at the temperature of 100-400 ℃ for 1-5 hours to obtain the target product.

8. The method for preparing polyether calcium phosphate quantum dots according to claim 7, wherein the deionized water: the weight ratio (w/w) of ethanol was (2:1) - (10: 1).

Technical Field

The invention relates to the technical field of petrochemical industry, relates to a quantum dot and a preparation method thereof, and particularly relates to a polyether calcium phosphate quantum dot and a preparation method thereof.

Background

Since the quantum dots are separated for the first time in 2004, researchers are concerned, particularly in recent years, the research on the quantum dots is very active, and the quantum dots can show potential application values in the fields of biological imaging, fluorescence sensing, organic photovoltaics, light emitting diodes, material self-repair and the like due to unique fluorescence characteristics. Quantum dots are generally extracted from mixtures of lead, cadmium and silicon, but these materials are generally toxic and environmentally hazardous, so scientists have begun extracting quantum dots from a number of benign compounds.

In recent years, carbon quantum dots also exhibit excellent performance in terms of reduced wear and reduced friction. The Kangzheng project group utilizes the characteristic that carbon quantum dots have a graphite-shaped multilayer structure and CuSx is easy to form CuFeySx-y alloy with metal Fe to prepare the carbon quantum dot/CuSx nano composition, and the composition shows excellent wear resistance and self-repairing performance in lubricating oil. In a driving experiment, the black smoke of the original automobile exhaust is reduced and even disappears. In pursuit of a green, efficient synthesis process for lubricants, researchers have tried a variety of approaches. Yan Honghao project group invented ultrasonic process for preparing carbon quantum dot lubricant additive, said process uses PEG, urea and citric acid as raw material, and in-situ synthesizes carbon quantum dot lubricant, under the condition of that said lubricant doesn't contain other adjuvant, the friction coefficient can be reduced to 0.02, and the four-ball test wear-mark diameter is 0.55 mm. Polyethers (PAGs) are of great interest as a group V base oil (according to API rules) with excellent detergency, viscosity index and anti-friction properties.

Disclosure of Invention

The invention aims to provide a novel quantum dot, which has uniform particles, good dispersibility with water and oil, and good abrasion resistance in oil products.

The technical scheme adopted by the invention for solving the technical problems is as follows:

the polyether calcium phosphate quantum dot consists of polyether and calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

Further, the polyether calcium phosphate quantum dots, preferably the polyether, are selected from water-soluble polyether, water-insoluble polyether or oil-soluble polyether.

Further, the polyether calcium phosphate quantum dot is preferably a compound of the following general formula:

wherein m is 0 to 100, n is 0 to 100, m and n are not zero at the same time, and R is1Is C1~C30Of (a) an alkane. R2Is hydrogen or methyl, R3Is C2~C30Of (a) an alkane.

Further, the polyether calcium phosphate quantum dots, preferably R1Is C1~C10Of (a) an alkane.

Further, the polyether calcium phosphate quantum dots, preferably R3Is C2~C20Of (a) an alkane.

Further, the polyether calcium phosphate quantum dots preferably have particle diameters of less than 10 nm.

The preparation method of the polyether calcium phosphate quantum dot is characterized by comprising the following steps:

A. weighing the following raw materials: 40-50 parts of polyether, 40-50 parts of calcium hydroxide, 40-50 parts of phosphoric acid, a proper amount of deionized water and a proper amount of ethanol;

B. preparing calcium hydroxide into 0.01-2.0mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at 40 deg.C at 0.1-2.0 mL/min, and controlling Ca concentration during the addition process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 0.5-3 hours after the dropwise addition is finished to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid;

D. drying the viscous solid at the temperature of 100-400 ℃ for 1-5 hours to obtain the target product.

Further, the preparation method of the polyether calcium phosphate quantum dot preferably comprises the following steps of: the weight ratio (w/w) of ethanol was (2:1) - (10: 1).

The polyether calcium phosphate quantum dot combines polyether and calcium phosphate, calcium phosphate is used as a core, polyether is used as a particle structure of a shell, the quantum dot particles are uniform, the dispersibility with water and oil is good, and the wear resistance in oil products is good.

The compound has simple process, is green and environment-friendly, and is easy to realize industrialization.

Detailed Description

In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described in detail.

The polyether calcium phosphate quantum dot consists of polyether and calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

Further, the polyether calcium phosphate quantum dots, preferably the polyether, are selected from water-soluble polyether, water-insoluble polyether or oil-soluble polyether.

Further, the polyether calcium phosphate quantum dot is preferably a compound of the following general formula:

wherein m is 0 to 100, n is 0 to 100, m and n are not zero at the same time, and R is1Is C1~C30Of (a) an alkane. R2Is hydrogen or methyl, R3Is C2~C30Of (a) an alkane.

Further, the polyether calcium phosphate quantum dots, preferably R1Is C1~C10Of (a) an alkane.

Further, the polyether calcium phosphate quantum dots, preferably R3Is C2~C20Of (a) an alkane.

Further, the polyether calcium phosphate quantum dots preferably have particle diameters of less than 10 nm.

A preparation method of polyether quantum dots comprises the following steps:

A. weighing the following raw materials: 40-50 parts of polyether, 40-50 parts of calcium hydroxide, 40-50 parts of phosphoric acid, a proper amount of deionized water and a proper amount of ethanol;

in the invention, the proper amount of deionized water and the proper amount of ethanol refer to the following components: the specific amount of deionized water and ethanol is consistent with the weight and concentration of calcium hydroxide, and is related to the ratio of deionized water to ethanol, and is not limited herein.

B. Preparing calcium hydroxide into a 0.01-2.0mol/L deionized water-ethanol solution, wherein the deionized water: the weight ratio (w/w) of ethanol is 2:1-10: 1. Adding phosphoric acid and polyether into calcium hydroxide solution at 40 deg.C at a rate of 0.1-2.0 mL/min, and controlling Ca during the addition process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 0.5-3 hours after the dropwise addition is finished to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid;

D. drying the viscous solid at the temperature of 100-400 ℃ for 1-5 hours to obtain the target product.

Further, the preparation method of the polyether calcium phosphate quantum dot,

the following is a detailed description of specific examples:

example 1, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 40 parts of polyether, 40 parts of calcium hydroxide, 40 parts of phosphoric acid, 3300 parts of deionized water and 700 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.01mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 0.1 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 0.5 hour after finishing dripping to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 100 ℃ for 1 hour to give the product of example 1.

Example 2, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 45 parts of polyether, 45 parts of calcium hydroxide, 45 parts of phosphoric acid, 80 parts of deionized water and 10 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 2.0mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 2.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 3 hours after the dropwise addition is finished to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 400 ℃ for 5 hours to give the product of example 2.

Example 3, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 50 parts of polyether, 50 parts of calcium hydroxide, 50 parts of phosphoric acid, 100 parts of deionized water and 10 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 1.0mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.5 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 1 hour after finishing the dropwise addition to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 350 ℃ for 1-5 hours to give the product of example 3.

Example 4, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 42 parts of polyether, 40 parts of calcium hydroxide, 40 parts of phosphoric acid, 640 parts of deionized water and 160 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.05mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 0.5 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 1.5 hours after the dropwise addition is finished to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 200 ℃ for 1-5 hours to give the product of example 4.

Example 5, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 48 parts of polyether, 45 parts of calcium hydroxide, 45 parts of phosphoric acid, 200 parts of deionized water and 25 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.2mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 0.5 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 300 ℃ for 3 hours to give the product of example 5.

Example 6, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 42 parts of polyether, 42 parts of calcium hydroxide, 42 parts of phosphoric acid, 60 parts of deionized water and 20 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.5mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.2 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 260 ℃ for 5 hours to give the product of example 6.

Example 7, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 50 parts of polyether, 40 parts of calcium hydroxide, 40 parts of phosphoric acid, 15 parts of deionized water and 5 parts of ethanol; wherein the polyether structure is:

B. preparing a calcium hydroxide raw material into a 1.8mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 2.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 1 hour after finishing the dropwise addition to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 400 ℃ for 2.5 hours to give the product of example 7.

Example 8, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 45 parts of polyether, 45 parts of calcium hydroxide, 45 parts of phosphoric acid, 130 parts of deionized water and 20 parts of ethanol; wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.3mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.5 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of the solution to the reaction solution at 3:2, and continuously reacting for 1.5 hours after the dropwise addition is finished to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 350 ℃ for 2 hours to give the product of example 8.

Example 9, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 44 parts of polyether, 42 parts of calcium hydroxide, 42 parts of phosphoric acid, 580 parts of deionized water and 120 parts of ethanol;

wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.06mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.5 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2 hours after finishing dripping to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 150 ℃ for 1-5 hours to give the product of example 9.

Example 10, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 46 parts of polyether, 45 parts of calcium hydroxide, 45 parts of phosphoric acid, 26 parts of deionized water and 13 parts of ethanol;

wherein the polyether structure is:

B. preparing a calcium hydroxide raw material into a 1.2mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.5 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 0.5 hour after finishing dripping to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 320 ℃ for 2.5 hours to give the product of example 10.

Example 11, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 50 parts of polyether, 45 parts of calcium hydroxide, 45 parts of phosphoric acid, 50 parts of deionized water and 13 parts of ethanol;

wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 2.0mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 2.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 350 ℃ for 4.0 hours to give the product of example 11.

Example 12, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 45 parts of polyether, 40 parts of calcium hydroxide, 40 parts of phosphoric acid, 100 parts of deionized water and 20 parts of ethanol;

wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.5mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 300 ℃ for 4.0 hours to give the product of example 12.

Example 13, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 45 parts of polyether, 35 parts of calcium hydroxide, 35 parts of phosphoric acid, 200 parts of deionized water and 20 parts of ethanol;

wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.5mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 300 ℃ for 4.0 hours to give the product of example 13.

Example 14, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 48 parts of polyether, 42 parts of calcium hydroxide, 42 parts of phosphoric acid, 200 parts of deionized water and 50 parts of ethanol;

wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.5mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 300 ℃ for 4.0 hours to give the product of example 14.

Example 15, a polyether calcium phosphate quantum dot is: polyetherAnd calcium phosphate, wherein the polyether is a shell layer, and the calcium phosphate is a core.

The preparation method of the polyether calcium phosphate quantum dot comprises the following steps:

A. weighing the following raw materials: 45 parts of polyether, 35 parts of calcium hydroxide, 35 parts of phosphoric acid, 200 parts of deionized water and 20 parts of ethanol;

wherein the polyether structure is:

B. preparing calcium hydroxide raw material into 0.5mol/L deionized water-ethanol solution, adding phosphoric acid and polyether into the calcium hydroxide solution at the same time at the rate of 1.0 mL/min at the temperature of 40 ℃, and controlling Ca all the time in the adding process2+:PO3 3-Keeping the molar ratio of 3:2, and continuously reacting for 2.5 hours after finishing the dropwise adding to obtain a solution 1;

C. filtering the solution 1, and removing the solvent to obtain a viscous solid 1;

D. the viscous solid 1 was dried at 300 ℃ for 4.0 hours to give the product of example 15.

Comparative experiment:

selecting the existing commercial quantum dots: ZnCdS/ZnS quantum dots, CdSe/ZnS quantum dots, CdS quantum dots, Cu and Mn co-doped quantum dots and graphene quantum dots.

1. Dispersibility test (particle size distribution method): the dispersibility was examined by measuring the particle size distribution using dynamic light scattering from a Zeta-potentiostat. 50ppm of quantum dots are added into 6 ml of solvent, the mixture is stirred for 60 minutes by using a homogenizer under the condition of 10000 revolutions per minute, and the dispersion condition of the solution is observed. The products of examples 1-15 of the present invention were tested for dispersibility with the existing commercial products as described above, with the following results:

TABLE 1 results of dispersibility experiments

From the dispersibility experiment, the product of the invention has better dispersibility in PAO4 base oil, deionized water and glycol, and the comparative example can not form good dispersibility in PAO4, deionized water and glycol at the same time compared with the product of the invention, wherein quantum dots containing metal particles have good dispersibility in PAO4, but have poor dispersibility in deionized water and glycol, and graphene quantum dots containing carbon only have good dispersibility in water and have poor dispersibility in PAO4 and glycol. Thus limiting its scope of application.

2. Abrasion resistance test (four-ball method):

preparation of a test sample: 1% quantum dot additive was added to PAO4 and stirred for 30 minutes.

The four-ball experimental conditions were: ASTM D2783 and D2596 rotating speed 1770r/min, time 10 s; the characteristic indexes are PB and PD values respectively, and the smaller the data is, the better the wear resistance is represented.

The products of examples 1-15 of the present invention were tested against the existing commercial products as described above for abrasion resistance, with the following specific results:

TABLE 2 abrasion resistance test

From the analysis of the maximum non-seizing load and sintering load data, the data of the product of the invention is obviously superior to that of a comparison sample, and the product has better abrasion resistance and extreme pressure property.

3. Cooling efficiency experiment:

preparation of a test sample: 1.5% quantum dot additive was added to deionized water and stirred for 30 minutes.

The cooling efficiency tests of the products of examples 1 to 15 of the present invention and the existing commercial products described above showed the following results:

TABLE 3 Cooling efficiency experiment

In the aspect of cooling efficiency, the product has good heat conductivity coefficient and hot melting; the comparative product is insoluble in water and therefore has a low thermal conductivity.

4. Particle range: the particle size of the product was tested by a nanometer particle sizer and transmission electron microscope.

The particle size of the products of examples 1-15 of the present invention was tested with the existing commercial product as described above, with the following specific results:

TABLE 4 Quantum dot particle size

Particle size range (nm)
Example 1 product 0.6-5.2
EXAMPLE 2 product 0.8-5.0
EXAMPLE 3 product 1.2-4.3
EXAMPLE 4 product 0.6-4.2
EXAMPLE 5 product 0.8-5.3
Example 6 product 1.6-5.9
Example 7 product 0.9-5.1
EXAMPLE 8 product 1.0-5.2
Example 9 product 0.7-4.9
EXAMPLE 10 product 0.9-5.0
EXAMPLE 11 product 1.0-4.9
EXAMPLE 12 product 0.7-4.8
EXAMPLE 13 product 1.1-5.1
EXAMPLE 14 product 0.8-5.1
EXAMPLE 15 product 0.6-4.8
ZnCdS/ZnS quantum dots 2.5-10.2
CdSe/ZnS quantum dots 2.8-10.1
CdS quantum dots 3.8-10.2
Cu and Mn codoped quantum dot 5.6-11.2
Graphene quantum dots 6.2-12.3

The product of the invention has smaller and narrower particle size distribution, can fully play the quantum dot effect and can be applied to more fields.

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