CN113104879A

CN113104879A - Method for preparing strontium fluoride crystal

Info

Publication number: CN113104879A
Application number: CN202110495716.3A
Authority: CN
Inventors: 曹译蕾; 钟学明; 李珊; 杨旭芳; 陈丹婷; 丁练; 李华
Original assignee: Nanchang Hangkong University
Current assignee: Nanchang Hangkong University
Priority date: 2021-05-07
Filing date: 2021-05-07
Publication date: 2021-07-13

Abstract

The invention relates to a method for preparing strontium fluoride crystals, which takes strontium chloride as a strontium source reactant, ammonium fluoride or sodium fluoride as a fluorine source reactant and glycine as a biological regulating agent to prepare the strontium fluoride crystals. Strontium chloride, ammonium fluoride or sodium fluoride and glycine solution are added into a communicated reactor provided with a left ear groove, a right ear groove, a left baffle plate, a middle baffle plate, a right baffle plate, and a product is filtered, washed and dried after the reaction is finished, so that strontium fluoride crystals are obtained. The strontium fluoride crystal prepared by the method has the purity of 99.0-99.9 percent, the yield of 99.0-99.9 percent and high purity and crystallinity. The method has the characteristics of simple flow, mild reaction conditions, low energy consumption and cost and the like.

Description

Method for preparing strontium fluoride crystal

Technical Field

The invention relates to a method for preparing strontium fluoride crystals, in particular to a method for preparing strontium fluoride crystals by a bionic method, wherein strontium chloride is taken as a strontium source reactant, ammonium fluoride or sodium fluoride is taken as a fluorine source reactant, and glycine is taken as a biological regulating agent. The invention relates to the preparation of strontium fluoride crystal in the technical field.

Background

The strontium fluoride crystal has good optical performance, anion conductivity and mechanical performance, is an extremely important functional material, and is widely applied to the fields of optical fiber communication, microelectronics, laser, photoelectrons, optics, solar energy, biology and the like. The existing preparation method of strontium fluoride crystal has the defects of high energy consumption, complex process and high cost.

In order to overcome the defects of high energy consumption, complex process and high cost of the preparation method of the strontium fluoride crystal, the strontium fluoride crystal is prepared by a bionic method by taking strontium chloride as a strontium source reactant, ammonium fluoride or sodium fluoride as a fluorine source reactant and glycine as a biological regulator.

Disclosure of Invention

Aiming at the defects of high energy consumption, complex process and high cost of the existing preparation method of the strontium fluoride crystal, the invention provides the preparation method of the strontium fluoride crystal, which has the advantages of mild reaction condition, low energy consumption, high purity, simple process and low cost.

The invention relates to a method for preparing strontium fluoride crystals, which takes strontium chloride as a strontium source reactant, ammonium fluoride or sodium fluoride as a fluorine source reactant and glycine as a biological regulating agent to react in a communicating reactor to prepare the strontium fluoride crystals. The specific technical scheme is as follows:

the communicating reactor is internally provided with a left ear groove, a right ear groove, a left baffle plate, a middle baffle plate, a right baffle plate, a left lower communicating port, a middle upper communicating port and a right lower communicating port; the left ear groove and the right ear groove are respectively arranged on the inner sides of the left side surface and the right side surface of the communicating reactor, and the upper edges of the left ear groove and the right ear groove are 10 cm lower than the upper edge of the communicating reactor and are used for storing reaction materials; the left baffle plate, the middle baffle plate and the right baffle plate separate the communicating reactor into four independent reaction zones, and the four independent reaction zones are communicated through a left lower communicating port, a middle upper communicating port and a right lower communicating port.

In a communicating reactor, according to the molar ratio of strontium to fluorine = 1: 2.10-1: 2.20, adding strontium chloride into a left ear tank, and adding ammonium fluoride or sodium fluoride into a right ear tank. Then adding a glycine solution with the mass percentage concentration of 0.10-0.20% into the communicating reactor, so that the liquid level of the glycine solution is 1 cm higher than the upper edges of the left ear tank and the right ear tank, and the reactants in the left ear tank and the right ear tank are communicated through the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal.

The invention has the beneficial effects that: 1) the preparation of the strontium fluoride crystal is completed at room temperature, and the reaction condition is mild and safe. 2) The reaction is carried out at room temperature, and the energy consumption is low. 3) The yield of the strontium fluoride crystal is high and reaches 99.0 to 99.9 percent. 4) The purity of the strontium fluoride crystal is high, and the purity of the strontium fluoride crystal is 99.0-99.9%. 6) The strontium fluoride crystal has high crystallinity and complete crystal development. 7) The preparation cost is low. The reaction device is simple, the operation is simple and convenient, and the reaction condition is mild.

Drawings

FIG. 1: XRD characterization results of the strontium fluoride crystal prepared by the invention. Comparing the XRD spectrogram of the strontium fluoride crystal prepared by the invention with a standard spectrogram card JCPDS number 06-0262 of the strontium fluoride crystal, the XRD characteristic peak position of the strontium fluoride crystal prepared by the invention is completely consistent with the standard spectrogram, and no impurity peak exists, so that the prepared product is proved to be the strontium fluoride crystal, and the product has no impurity and high purity. As can be seen from FIG. 1, the strontium fluoride prepared by the invention has good crystal development and high crystallinity.

FIG. 2: schematic of the communicating reactor of the present invention. In FIG. 2, A is a left ear tank installed inside the left side of the communicating reactor, the upper edge of the left ear tank is 10 cm lower than the upper edge of the reactor, and the left ear tank is used for containing reactants; b is a left baffle plate for blocking the upper part; c is a middle baffle plate for blocking the lower part; d is a right baffle plate for blocking the upper part; e is a right lug groove which is arranged at the inner side of the right side of the communicated reactor, the upper edge of the right lug groove is 10 cm lower than the upper edge of the reactor, and the right lug groove is used for containing reactants; f is a left lower communicating port used for communicating the lower part; g is an upper communicating port for communicating the upper part; h is a lower right communication port for communicating the lower part.

Detailed Description

A method for producing a strontium fluoride crystal according to the present invention will be further described with reference to the following examples.

Example 1

In a communicating reactor provided with 2 left ear grooves, 3 left, middle and right baffle plates, strontium and fluorine = 1: 2.15 according to molar ratio, strontium chloride is added into the left ear groove, and ammonium fluoride is added into the right ear groove. Then, a glycine solution containing 0.15% by mass of glycine at a concentration ratio was fed into the communicating reactor so that the liquid level of the glycine solution was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated by the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal. The yield of strontium fluoride crystals was 99.5% and the purity was 99.6%.

Example 2

In a communicating reactor provided with 2 left ear grooves, 3 left, middle and right baffle plates, strontium and fluorine = 1: 2.10 according to molar ratio, strontium chloride is added into the left ear groove, and ammonium fluoride is added into the right ear groove. Then, a glycine solution containing 0.10% by mass of glycine at a ratio of concentration to concentration was fed into the communicating reactor so that the liquid level of the glycine solution was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated by the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal. The yield of strontium fluoride crystals was 99.0% and the purity was 99.9%.

Example 3

In a communicating reactor provided with 2 left ear grooves, 3 left, middle and right baffle plates, strontium and fluorine = 1: 2.20 according to molar ratio, strontium chloride is added into the left ear groove, and ammonium fluoride is added into the right ear groove. Then, a glycine solution containing 0.20% by mass of glycine at a concentration ratio was fed into the communicating reactor so that the liquid level of the glycine solution was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated by the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal. The yield of strontium fluoride crystals was 99.9% and the purity was 99.3%.

Example 4

In a communicating reactor provided with 2 left ear grooves, 3 left, middle and right baffle plates, strontium and fluorine = 1: 2.15 according to molar ratio, strontium chloride is added into the left ear groove, and sodium fluoride is added into the right ear groove. Then, a glycine solution containing 0.15% by mass of glycine at a concentration ratio was fed into the communicating reactor so that the liquid level of the glycine solution was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated by the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal. The yield of strontium fluoride crystals was 99.6% and the purity was 99.5%.

Example 5

In a communicating reactor provided with 2 left ear grooves, 3 left, middle and right baffle plates, strontium and fluorine = 1: 2.10 according to molar ratio, strontium chloride is added into the left ear groove, and sodium fluoride is added into the right ear groove. Then, a glycine solution containing 0.10% by mass of glycine at a ratio of concentration to concentration was fed into the communicating reactor so that the liquid level of the glycine solution was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated by the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal. The yield of strontium fluoride crystals was 99.0% and the purity was 99.9%.

Example 6

In a communicating reactor provided with 2 left ear grooves, 3 left, middle and right baffle plates, strontium and fluorine = 1: 2.20 according to molar ratio, strontium chloride is added into the left ear groove, and sodium fluoride is added into the right ear groove. Then, a glycine solution containing 0.20% by mass of glycine at a concentration ratio was fed into the communicating reactor so that the liquid level of the glycine solution was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated by the mixture solution. Covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal. The yield of strontium fluoride crystals was 99.9% and the purity was 99.2%.

Claims

1. A method of preparing strontium fluoride crystals, comprising: the method takes strontium chloride as a strontium source reactant, ammonium fluoride or sodium fluoride as a fluorine source reactant and glycine as a biological regulating agent, and the strontium chloride, the ammonium fluoride or the sodium fluoride and the glycine react in a communicated reactor to prepare a strontium fluoride crystal; the specific technical scheme is as follows:

the communicating reactor is internally provided with a left ear groove, a right ear groove, a left baffle plate, a middle baffle plate, a right baffle plate, a left lower communicating port, a middle upper communicating port and a right lower communicating port; the left ear groove and the right ear groove are respectively arranged on the inner sides of the left side surface and the right side surface of the communicating reactor, and the upper edges of the left ear groove and the right ear groove are 10 cm lower than the upper edge of the communicating reactor and are used for storing reaction materials; the left baffle plate, the middle baffle plate and the right baffle plate divide the communicating reactor into four independent reaction zones, and the four independent reaction zones are communicated through a left lower communicating port, a middle upper communicating port and a right lower communicating port;

in a communicating reactor, according to the molar ratio of strontium to fluorine = 1: 2.10-1: 2.20, adding strontium chloride into a left ear groove, and adding ammonium fluoride or sodium fluoride into a right ear groove; then adding a glycine solution with the mass percentage concentration of 0.10-0.20% into the communicating reactor, so that the liquid level of the glycine solution is higher than the upper edges of the left ear tank and the right ear tank by 1 cm, and the reactants in the left ear tank and the right ear tank are communicated through the mixture solution; covering a cover on the communicating reactor, standing for reaction for 7 days, filtering, washing and drying the product at 105 ℃ for 1 h to obtain the strontium fluoride crystal.