Industrial preparation process of optical fluoride salt product

Abstract

The invention discloses an industrial preparation process of an optical-grade fluoride salt product, and relates to the technical field of fluoride salt products, and the industrial preparation process comprises the following steps: (1) obtaining a chloride salt solution; (2) obtaining an intermediate reaction solution; (3) obtaining a sodium fluoborate solution; (4) obtaining a mixed solution; (5) obtaining a reaction system; (6) obtaining a primary reaction material; (7) carrying out modification treatment on the primary reaction material to obtain an optical-grade fluoride salt product; the prepared optical-grade fluoride salt product can be applied to optical glass, and the stability performance of the optical glass can be greatly improved.

Description

Technical Field

[0001] The invention belongs to the technical field of fluoride salt products, in particular to an industrial preparation process of optical-grade fluoride salt products. Background Art

[0002] Optical grade fluoride salt products are a type of fluoride with special applications in the optical field. Optical grade fluoride salt products have a wide range of applications, including:

[0003] 1. Optical glass: Optical grade fluoride salts are widely used to manufacture various types of optical glass, such as lenses, prisms, filters, etc. They can improve the refractive index, dispersion and transmittance of glass, and improve the imaging quality and resolution of optical systems.

[0004] 2. Fiber optic communication: In the field of fiber optic communication, optical grade fluoride salts are used as one of the core raw materials for fiber optic preforms. By precisely controlling its composition and process conditions, high-quality optical fibers with high transmission efficiency, low loss and low dispersion can be produced.

[0005] 3. Optical crystals: Certain optical-grade fluoride salts can also be used as matrix materials for growing high-quality optical crystals. These crystals have broad application prospects in the fields of laser technology, nonlinear optics, etc.

[0006] With the continuous development of optical technology and the continuous expansion of its application fields, the market demand for optical-grade fluoride salts is also increasing year by year. In particular, its application in high-tech fields such as optoelectronics, optical communications, and laser technology has driven the rapid growth of the market.

[0007] As the demand for optical-grade fluoride salt products continues to increase, the performance requirements are also constantly improving, requiring them to provide better performance improvements for optical glass. Summary of the invention

[0008] The purpose of the present invention is to provide an industrial preparation process for an optical grade fluoride salt product to solve the deficiencies in the prior art.

[0009] The technical solution adopted by the present invention is as follows:

[0010] An industrial preparation process for an optical grade fluoride salt product comprises the following steps:

[0011] (1) adding chloride salt to deionized water, stirring and mixing until all the chloride salt is dissolved, to obtain a chloride salt solution;

[0012] (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 60-70° C., and stirring for 40-50 minutes to obtain an intermediate reaction solution;

[0013] Among them, the stirring speed is 200r / min;

[0014] (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution;

[0015] Among them, the stirring speed is 150r / min;

[0016] (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 78-80° C., and stirring for 2 hours to obtain a mixed solution;

[0017] Among them, the stirring speed is 150r / min;

[0018] (5) heating the obtained mixed solution to 160-170° C. in a reaction kettle under the protection of an inert atmosphere, stirring and keeping warm for 24-26 hours, and then cooling to room temperature to obtain a reaction system;

[0019] Among them, the stirring speed is 1000r / min;

[0020] (6) The obtained reaction system is subjected to high-speed centrifugation for 10 minutes, and then filtered, washed, and dried to obtain a preliminary reaction material;

[0021] Among them, the speed of high-speed centrifugal treatment is 8500r / min;

[0022] Among them, the drying temperature is 80°C and the drying time is 5 hours;

[0023] (7) The preliminary reaction material is modified to obtain an optical grade fluoride salt product.

[0024] As a further technical solution: the chloride salt in step (1) comprises a mixture of calcium chloride, manganese chloride and cerium chloride;

[0025] Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3;

[0026] The concentration of chloride solution is 3-5 mol / L.

[0027] As a further technical solution: the molar ratio of disodium ethylenediaminetetraacetate to chloride in step (2) is 1:2.

[0028] As a further technical solution: in step (3), the concentration of the sodium fluoroborate solution is 1.5-2.5 mol / L;

[0029] When the sodium fluoroborate solution is mixed with the intermediate reaction solution in step (4), the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:1.

[0030] As a further technical solution: the inert atmosphere in step (5) is either nitrogen or neon.

[0031] As a further technical solution: the modification treatment method of the preliminary reaction material is:

[0032] First, the preliminary reaction material is evenly dispersed in deionized water to obtain a preliminary reaction material dispersion;

[0033] Then, the obtained preliminary reaction material dispersion liquid is added into anhydrous ethanol, and ultrasonically dispersed for 10 minutes to obtain an alcohol dispersion liquid;

[0034] Prepare an ammonia solution with a mass concentration of 20%;

[0035] The pH of the alcohol dispersion was adjusted to 10-10.5 with an ammonia solution and allowed to stand for 20 minutes;

[0036] Then, ethyl orthosilicate is added to the alcohol dispersion, and the mixture is stirred at 25° C. for 5 hours. The mixture is then subjected to high-speed centrifugation for 10 minutes, filtered, and vacuum dried to obtain an optical grade fluoride salt product.

[0037] As a further technical solution: the mixing ratio of the preliminary reaction material and deionized water is 10-14g:120mL;

[0038] The volume ratio of the initial reaction material dispersion and anhydrous ethanol is 1:3.

[0039] As a further technical solution: the mass ratio of the preliminary reaction material to ethyl orthosilicate is 10:1-3.

[0040] As a further technical solution: the high-speed centrifugal treatment speed is 7500r / min.

[0041] As a further technical solution, the vacuum drying temperature is 55° C. and the time is 10 hours.

[0042] Beneficial effects:

[0043] The optical-grade fluoride salt product prepared by the invention can be applied to optical glass, and can greatly improve the stability performance of the optical glass.

[0044] The present invention mainly improves the comprehensive performance of the obtained fluoride salt product by modifying the initial reaction material, thereby improving the optical application performance of the fluoride salt product and broadening the application field of the product. By introducing a certain amount of cerium element into the fluoride salt product, the corrosion resistance of the optical glass can be further improved, and cerium fluoride has a lower light absorption coefficient, which can allow more light to pass through, thereby reducing light loss and improving the light transmittance of the optical glass.

[0045] By introducing the optical grade fluoride salt product prepared by the present invention, the light transmittance of optical glass can be greatly enhanced. Its main mechanism of action is that it can make the propagation of light in the optical glass smoother, greatly reducing the loss and scattering of light, thereby significantly improving the performance and quality of the optical glass and broadening the application range of the optical glass products after introduction.

[0046] In the manufacture of optical glass, the addition of the optical grade fluoride salt product prepared by the present invention can significantly improve the chemical corrosion resistance of the optical glass and effectively avoid the problem of discoloration of the optical glass during long-term use. This is of great significance for maintaining the stability and durability of the optical glass.

[0047] By introducing the fluoride salt product prepared by the present invention, it is evenly dispersed in the optical glass, which can effectively reduce the reflection of light on the surface of the optical glass. Especially in the application of glasses and automotive glass, this feature helps to reduce reflection and glare and improve visual comfort. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 Statistical chart of light transmittance of each group. DETAILED DESCRIPTION

[0049] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only 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.

[0050] Example 1

[0051] An industrial preparation process for an optical grade fluoride salt product comprises the following steps:

[0052] (1) adding chloride salt to deionized water, stirring and mixing until all dissolved, to obtain a chloride salt solution; the chloride salt includes: a mixture of calcium chloride, manganese chloride, and cerium chloride;

[0053] Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3;

[0054] The concentration of chloride solution is 3 mol / L.

[0055] (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 60° C., and stirring for 40 minutes to obtain an intermediate reaction solution;

[0056] The stirring speed is 200 r / min; the molar ratio of disodium ethylenediaminetetraacetic acid to chloride is 1:2.

[0057] (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution;

[0058] Wherein, the stirring speed is 150r / min; the concentration of sodium fluoroborate solution is 1.5mol / L;

[0059] (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 78° C., and stirring for 2 hours to obtain a mixed solution;

[0060] The stirring speed is 150 r / min; when the sodium fluoroborate solution is mixed with the intermediate reaction solution, the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:1.

[0061] (5) heating the obtained mixed solution to 160° C. in a reaction vessel under the protection of an inert atmosphere, stirring and keeping the mixture warm for 24 hours, and then cooling the mixture to room temperature to obtain a reaction system;

[0062] The stirring speed was 1000 r / min and the inert atmosphere was nitrogen.

[0063] (6) The obtained reaction system is subjected to high-speed centrifugation for 10 minutes, and then filtered, washed, and dried to obtain a preliminary reaction material;

[0064] Among them, the speed of high-speed centrifugal treatment is 8500r / min;

[0065] Among them, the drying temperature is 80°C and the drying time is 5 hours;

[0066] (7) modifying the initial reaction material to obtain an optical grade fluoride salt product;

[0067] The modification treatment method of the initial reaction material is as follows:

[0068] First, the preliminary reaction material is evenly dispersed in deionized water to obtain a dispersion of the preliminary reaction material; the mixing ratio of the preliminary reaction material and deionized water is 10 g: 120 mL;

[0069] The obtained reaction preliminary material dispersion was then added to anhydrous ethanol and ultrasonically dispersed for 10 minutes to obtain an alcohol dispersion; the volume ratio of the reaction preliminary material dispersion to anhydrous ethanol was 1:3.

[0070] Prepare an ammonia solution with a mass concentration of 20%;

[0071] The pH of the alcohol dispersion was adjusted to 10.0 using an ammonia solution and allowed to stand for 20 minutes;

[0072] Then, add tetraethyl orthosilicate to the alcohol dispersion, keep warm and stir at 25°C for 5 hours, then high-speed centrifuge for 10 minutes, filter, and vacuum dry to obtain an optical grade fluoride salt product; the mass ratio of the initial reaction material to tetraethyl orthosilicate is 10:1; the high-speed centrifuge speed is 7500r / min; the vacuum drying temperature is 55°C and the time is 10 hours.

[0073] Example 2

[0074] An industrial preparation process for an optical grade fluoride salt product comprises the following steps:

[0075] (1) adding chloride salt to deionized water, stirring and mixing until all dissolved, to obtain a chloride salt solution; the chloride salt includes: a mixture of calcium chloride, manganese chloride, and cerium chloride;

[0076] Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3;

[0077] The concentration of chloride solution is 4 mol / L.

[0078] (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 65° C., and stirring for 40 minutes to obtain an intermediate reaction solution;

[0079] The stirring speed is 200 r / min; the molar ratio of disodium ethylenediaminetetraacetic acid to chloride is 1:2.

[0080] (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution;

[0081] Wherein, the stirring speed is 150r / min; the concentration of sodium fluoroborate solution is 1.84mol / L;

[0082] (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 79° C., and stirring for 2 hours to obtain a mixed solution;

[0083] The stirring speed is 150 r / min; when the sodium fluoroborate solution is mixed with the intermediate reaction solution, the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:1.

[0084] (5) heating the obtained mixed solution to 168° C. in a reaction vessel under the protection of an inert atmosphere, stirring and keeping the mixture warm for 25 hours, and then cooling the mixture to room temperature to obtain a reaction system;

[0085] The stirring speed was 1000 r / min and the inert atmosphere was nitrogen.

[0086] (6) The obtained reaction system is subjected to high-speed centrifugation for 10 minutes, and then filtered, washed, and dried to obtain a preliminary reaction material;

[0087] Among them, the speed of high-speed centrifugal treatment is 8500r / min;

[0088] Among them, the drying temperature is 80°C and the drying time is 5 hours;

[0089] (7) modifying the initial reaction material to obtain an optical grade fluoride salt product;

[0090] The modification treatment method of the initial reaction material is as follows:

[0091] First, the preliminary reaction material is evenly dispersed in deionized water to obtain a dispersion of the preliminary reaction material; the mixing ratio of the preliminary reaction material and deionized water is 12g:120mL;

[0092] The obtained reaction preliminary material dispersion was then added to anhydrous ethanol and ultrasonically dispersed for 10 minutes to obtain an alcohol dispersion; the volume ratio of the reaction preliminary material dispersion to anhydrous ethanol was 1:3.

[0093] Prepare an ammonia solution with a mass concentration of 20%;

[0094] The pH of the alcohol dispersion was adjusted to 10.2 using an ammonia solution and allowed to stand for 20 minutes;

[0095] Then, add tetraethyl orthosilicate to the alcohol dispersion, keep warm and stir at 25°C for 5 hours, then high-speed centrifuge for 10 minutes, filter, and vacuum dry to obtain an optical grade fluoride salt product; the mass ratio of the initial reaction material to tetraethyl orthosilicate is 10:1.5; the high-speed centrifuge speed is 7500r / min; the vacuum drying temperature is 55°C and the time is 10 hours.

[0096] Example 3

[0097] An industrial preparation process for an optical grade fluoride salt product comprises the following steps:

[0098] (1) adding chloride salt to deionized water, stirring and mixing until all dissolved, to obtain a chloride salt solution; the chloride salt includes: a mixture of calcium chloride, manganese chloride, and cerium chloride;

[0099] Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3;

[0100] The concentration of chloride solution is 3.8 mol / L.

[0101] (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 68° C., and stirring for 45 minutes to obtain an intermediate reaction solution;

[0102] The stirring speed is 200 r / min; the molar ratio of disodium ethylenediaminetetraacetic acid to chloride is 1:2.

[0103] (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution;

[0104] Wherein, the stirring speed is 150r / min; the concentration of sodium fluoroborate solution is 1.95mol / L;

[0105] (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 78° C., and stirring for 2 hours to obtain a mixed solution;

[0106] The stirring speed is 150 r / min; when the sodium fluoroborate solution is mixed with the intermediate reaction solution, the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:1.

[0107] (5) heating the obtained mixed solution to 160° C. in a reaction vessel under the protection of an inert atmosphere, stirring and keeping the mixture warm for 25 hours, and then cooling the mixture to room temperature to obtain a reaction system;

[0108] The stirring speed was 1000 r / min and the inert atmosphere was nitrogen.

[0109] (6) The obtained reaction system is subjected to high-speed centrifugation for 10 minutes, and then filtered, washed, and dried to obtain a preliminary reaction material;

[0110] Among them, the speed of high-speed centrifugal treatment is 8500r / min;

[0111] Among them, the drying temperature is 80°C and the drying time is 5 hours;

[0112] (7) modifying the initial reaction material to obtain an optical grade fluoride salt product;

[0113] The modification treatment method of the initial reaction material is as follows:

[0114] First, the preliminary reaction material is evenly dispersed in deionized water to obtain a preliminary reaction material dispersion; the mixing ratio of the preliminary reaction material and deionized water is 13g:120mL;

[0115] The obtained reaction preliminary material dispersion was then added to anhydrous ethanol and ultrasonically dispersed for 10 minutes to obtain an alcohol dispersion; the volume ratio of the reaction preliminary material dispersion to anhydrous ethanol was 1:3.

[0116] Prepare an ammonia solution with a mass concentration of 20%;

[0117] The pH of the alcohol dispersion was adjusted to 10.3 with an ammonia solution and allowed to stand for 20 minutes;

[0118] Then, add tetraethyl orthosilicate to the alcohol dispersion, keep warm and stir at 25°C for 5 hours, then high-speed centrifuge for 10 minutes, filter, and vacuum dry to obtain an optical grade fluoride salt product; the mass ratio of the initial reaction material to tetraethyl orthosilicate is 10:2.2; the high-speed centrifuge speed is 7500r / min; the vacuum drying temperature is 55°C and the time is 10 hours.

[0119] Example 4

[0120] An industrial preparation process for an optical grade fluoride salt product comprises the following steps:

[0121] (1) adding chloride salt to deionized water, stirring and mixing until all dissolved, to obtain a chloride salt solution; the chloride salt includes: a mixture of calcium chloride, manganese chloride, and cerium chloride;

[0122] Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3;

[0123] The concentration of chloride solution is 4.2 mol / L.

[0124] (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 68° C., and stirring for 45 minutes to obtain an intermediate reaction solution;

[0125] The stirring speed is 200 r / min; the molar ratio of disodium ethylenediaminetetraacetic acid to chloride is 1:2.

[0126] (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution;

[0127] Wherein, the stirring speed is 150r / min; the concentration of sodium fluoroborate solution is 2.1mol / L;

[0128] (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 79° C., and stirring for 2 hours to obtain a mixed solution;

[0129] The stirring speed is 150 r / min; when the sodium fluoroborate solution is mixed with the intermediate reaction solution, the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:1.

[0130] (5) heating the obtained mixed solution to 165° C. in a reaction vessel under the protection of an inert atmosphere, stirring and keeping the mixture warm for 25 hours, and then cooling the mixture to room temperature to obtain a reaction system;

[0131] The stirring speed was 1000 r / min and the inert atmosphere was nitrogen.

[0132] (6) The obtained reaction system is subjected to high-speed centrifugation for 10 minutes, and then filtered, washed, and dried to obtain a preliminary reaction material;

[0133] Among them, the speed of high-speed centrifugal treatment is 8500r / min;

[0134] Among them, the drying temperature is 80°C and the drying time is 5 hours;

[0135] (7) modifying the initial reaction material to obtain an optical grade fluoride salt product;

[0136] The modification treatment method of the initial reaction material is as follows:

[0137] First, the preliminary reaction material is evenly dispersed in deionized water to obtain a preliminary reaction material dispersion; the mixing ratio of the preliminary reaction material and deionized water is 11g:120mL;

[0138] The obtained reaction preliminary material dispersion was then added to anhydrous ethanol and ultrasonically dispersed for 10 minutes to obtain an alcohol dispersion; the volume ratio of the reaction preliminary material dispersion to anhydrous ethanol was 1:3.

[0139] Prepare an ammonia solution with a mass concentration of 20%;

[0140] The pH of the alcohol dispersion was adjusted to 10.4 using an ammonia solution and allowed to stand for 20 minutes;

[0141] Then, add tetraethyl orthosilicate to the alcohol dispersion, keep warm and stir at 25°C for 5 hours, then high-speed centrifuge for 10 minutes, filter, and vacuum dry to obtain an optical grade fluoride salt product; the mass ratio of the initial reaction material to tetraethyl orthosilicate is 10:2.5; the high-speed centrifuge speed is 7500r / min; the vacuum drying temperature is 55°C and the time is 10 hours.

[0142] Example 5

[0143] An industrial preparation process for an optical grade fluoride salt product comprises the following steps:

[0144] (1) adding chloride salt to deionized water, stirring and mixing until all dissolved, to obtain a chloride salt solution; the chloride salt includes: a mixture of calcium chloride, manganese chloride, and cerium chloride;

[0145] Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3;

[0146] The concentration of chloride solution is 5 mol / L.

[0147] (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 70° C., and stirring for 50 minutes to obtain an intermediate reaction solution;

[0148] The stirring speed is 200 r / min; the molar ratio of disodium ethylenediaminetetraacetic acid to chloride is 1:2.

[0149] (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution;

[0150] Wherein, the stirring speed is 150r / min; the concentration of sodium fluoroborate solution is 2.5mol / L;

[0151] (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 80° C., and stirring for 2 hours to obtain a mixed solution;

[0152] The stirring speed is 150 r / min; when the sodium fluoroborate solution is mixed with the intermediate reaction solution, the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:1.

[0153] (5) heating the obtained mixed solution to 170° C. in a reaction vessel under the protection of an inert atmosphere, keeping the mixture warm and stirring for 26 hours, and then cooling it to room temperature to obtain a reaction system;

[0154] The stirring speed was 1000 r / min and the inert atmosphere was nitrogen.

[0155] (6) The obtained reaction system is subjected to high-speed centrifugation for 10 minutes, and then filtered, washed, and dried to obtain a preliminary reaction material;

[0156] Among them, the speed of high-speed centrifugal treatment is 8500r / min;

[0157] Among them, the drying temperature is 80°C and the drying time is 5 hours;

[0158] (7) modifying the initial reaction material to obtain an optical grade fluoride salt product;

[0159] The modification treatment method of the initial reaction material is as follows:

[0160] First, the preliminary reaction material is evenly dispersed in deionized water to obtain a preliminary reaction material dispersion; the mixing ratio of the preliminary reaction material and deionized water is 14g:120mL;

[0161] The obtained reaction preliminary material dispersion was then added to anhydrous ethanol and ultrasonically dispersed for 10 minutes to obtain an alcohol dispersion; the volume ratio of the reaction preliminary material dispersion to anhydrous ethanol was 1:3.

[0162] Prepare an ammonia solution with a mass concentration of 20%;

[0163] The pH of the alcohol dispersion was adjusted to 10.5 with an ammonia solution and allowed to stand for 20 minutes;

[0164] Then, add tetraethyl orthosilicate to the alcohol dispersion, keep warm and stir at 25°C for 5 hours, then high-speed centrifuge for 10 minutes, filter, and vacuum dry to obtain an optical grade fluoride salt product; the mass ratio of the initial reaction material to tetraethyl orthosilicate is 10:3; the high-speed centrifuge speed is 7500r / min; the vacuum drying temperature is 55°C and the time is 10 hours.

[0165] Comparative Example 1:

[0166] The difference from Example 1 is that the preliminary reaction material is not subjected to modification treatment.

[0167] Comparative Example 2:

[0168] The difference from Example 1 is that no cerium chloride is added to the chloride salt.

[0169] test:

[0170] Glass sample: The composition range of borosilicate optical glass is (wt%): B2O3: 20.3%, A12O3: 8.36%, Example / Comparative Example sample 0.5%, and the rest is SiO2;

[0171] Blank glass sample: composition range is (wt%): B2O3: 20.3%, A12O3: 8.36%, the rest is SiO 2；

[0172] The preparation parameters of each group of samples were the same, and the sample glass with a thickness of 2 mm was obtained;

[0173] Chemical stability

[0174] The glass samples of each group were immersed in 50mL / L HCL solution and 50g / L NaOH solution in a water bath at 95℃ for heating (6h for acid and 4h for alkali). After taking out the samples, the impurities on the surface of the glass blocks were washed with deionized water and alcohol. After drying, the samples were weighed and the weight loss per unit area (mg / dm 2 ), compare the chemical stability of each group;

[0175] Table 1

[0176]

[0177] It can be seen from Table 1 that the optical grade fluoride salt product prepared by the present invention is introduced into optical glass, which can greatly improve the chemical stability of the optical glass.

[0178] Continuing the above test, taking Example 1 as the basic sample, the effects of different addition amounts on the alkali resistance of optical glass are compared:

[0179] Table 2

[0180]

[0181]

[0182] It can be seen from Table 2 that with the increase in the amount of sample added, the alkali resistance of the optical glass continues to increase, and will decrease slightly after exceeding a certain concentration.

[0183] The transmittance of the optical glass of the embodiment and the comparative example samples was tested using a Lambda950 visible ultraviolet near infrared spectrophotometer: the test wavelength range was 300-800nm, and the step length was 10nm;

[0184] Table 3

[0185]

[0186]

[0187] It can be seen from Table 3 that the light transmittance of optical glass can be greatly improved after the product of the present invention is introduced.

[0188] The above description is only a preferred embodiment of the present invention, but the present invention is not limited to the scope of implementation shown. Any changes made according to the concept of the present invention, or modifications to equivalent embodiments with equivalent changes, which still do not exceed the description, should be within the protection scope of the present invention.

Claims

1. An industrial preparation process for an optical grade fluoride salt product, characterized in that: The following steps are involved: (1) adding chloride salt to deionized water, stirring and mixing until all the chloride salt is dissolved, to obtain a chloride salt solution; (2) adding disodium ethylenediaminetetraacetate to the chloride solution, adjusting the temperature to 60-70° C., and stirring for 40-50 minutes to obtain an intermediate reaction solution; Among them, the stirring speed is 200r / min; (3) adding sodium fluoroborate to deionized water, stirring and mixing until all the sodium fluoroborate is dissolved, to obtain a sodium fluoroborate solution; Among them, the stirring speed is 150r / min; (4) adding the obtained sodium fluoroborate solution dropwise to the intermediate reaction solution, adjusting the temperature to 78-80° C., and stirring for 2 hours to obtain a mixed solution; Among them, the stirring speed is 150r / min; (5) heating the obtained mixed solution to 160-170° C. in a reaction kettle under the protection of an inert atmosphere, stirring and keeping warm for 24-26 hours, and then cooling to room temperature to obtain a reaction system; Among them, the stirring speed is 1000r / min; (6) The obtained reaction system is subjected to high-speed centrifugation for 10 min, and then filtered, washed, and dried to obtain a preliminary reaction material; Among them, the speed of high-speed centrifugal treatment is 8500r / min; Among them, the drying temperature is 80°C and the drying time is 5 hours; (7) The preliminary reaction material is modified to obtain an optical grade fluoride salt product.

2. The industrial preparation process of an optical grade fluoride salt product according to claim 1, characterized in that: The chloride salt in step (1) comprises a mixture of calcium chloride, manganese chloride and cerium chloride; Wherein, the molar ratio of calcium chloride, manganese chloride and cerium chloride is 10:3:0.3; The concentration of chloride salt solution is 3-5 mol / L.

3. The industrial preparation process of an optical grade fluoride salt product according to claim 1, characterized in that: The molar ratio of disodium ethylenediaminetetraacetate to chloride in step (2) is 1:

2.

4. The industrial preparation process of an optical grade fluoride salt product according to claim 1, characterized in that: In step (3), the concentration of the sodium fluoroborate solution is 1.5-2.5 mol / L; When the sodium fluoroborate solution is mixed with the intermediate reaction solution in step (4), the volume ratio of the sodium fluoroborate solution to the chloride solution is 1:

1.

5. The industrial preparation process of an optical grade fluoride salt product according to claim 1, characterized in that: The inert atmosphere in step (5) is either nitrogen or neon.

6. The industrial preparation process of an optical grade fluoride salt product according to claim 1, characterized in that: The modification treatment method of the preliminary reaction material is as follows: First, the preliminary reaction material is evenly dispersed in deionized water to obtain a preliminary reaction material dispersion; The obtained preliminary reaction material dispersion liquid is then added to anhydrous ethanol and dispersed by ultrasonic for 10 minutes to obtain an alcohol dispersion liquid; Prepare an ammonia solution with a mass concentration of 20%; The pH of the alcohol dispersion was adjusted to 10-10.5 with an ammonia solution and allowed to stand for 20 minutes; Then, ethyl orthosilicate is added to the alcohol dispersion, and the mixture is stirred at 25° C. for 5 hours. The mixture is then subjected to high-speed centrifugation for 10 minutes, filtered, and vacuum dried to obtain an optical grade fluoride salt product.

7. The industrial preparation process of an optical grade fluoride salt product according to claim 6, characterized in that: The mixing ratio of the preliminary reaction material and deionized water is 10-14g:120mL; The volume ratio of the initial reaction material dispersion and anhydrous ethanol is 1:

3.

8. The industrial preparation process of an optical grade fluoride salt product according to claim 6, characterized in that: The mass ratio of the preliminary reaction material to ethyl orthosilicate is 10:1-3.

9. The industrial preparation process of an optical grade fluoride salt product according to claim 6, characterized in that: The high-speed centrifugal treatment speed is 7500r / min.

10. The industrial preparation process of an optical grade fluoride salt product according to claim 6, characterized in that: The vacuum drying temperature is 55° C. and the time is 10 hours.

Images